Sample records for extract dilution analysis

  1. Characterization of the key aroma compounds in beef extract using aroma extract dilution analysis. (United States)

    Takakura, Yukiko; Sakamoto, Tomohiro; Hirai, Sachi; Masuzawa, Takuya; Wakabayashi, Hidehiko; Nishimura, Toshihide


    Aroma extract dilution analysis (AEDA) of an ether extract prepared from beef extract (BE) and subsequent identification experiments led to the determination of seven aroma-active compounds in the flavor dilution (FD) factor range of 32-128. Omission experiments to select the most aroma-active compounds from the seven aroma compounds suggested that 2,3,5-trimethyl pyrazine, 1-octen-3-ol, 3-methylbutanoic acid, and 4-hydroxy-2,5-dimethyl-3(2H)-furanone were the main active compounds contributing to the aroma of BE. Aroma recombination, addition, and omission experiments of the four aroma compounds in taste-reconstituted BE showed that each compound had an individual aroma profile. A comparison of the overall aroma between this recombination mixture and BE showed a high similarity, suggesting that the key aroma compounds had been identified successfully.

  2. Identification of Key Odorants in Withering-Flavored Green Tea by Aroma Extract Dilution Analysis (United States)

    Mizukami, Yuzo; Yamaguchi, Yuichi

    This research aims to identify key odorants in withering-flavored green tea. Application of the aroma extract dilution analysis using the volatile fraction of green tea and withering-flavored green tea revealed 25 and 35 odor-active peaks with the flavor dilution factors of≥4, respectively. 4-mercapto-4-methylpentan-2-one, (E)-2-nonenal, linalool, (E,Z)-2,6-nonadienal and 3-methylnonane-2,4-dione were key odorants in green tea with the flavor dilution factor of≥16. As well as these 5 odorants, 1-octen-3-one, β-damascenone, geraniol, β-ionone, (Z)-methyljasmonate, indole and coumarine contributed to the withering flavor of green tea.

  3. Characterization of typical potent odorants in cola-flavored carbonated beverages by aroma extract dilution analysis. (United States)

    Lorjaroenphon, Yaowapa; Cadwallader, Keith R


    The aroma-active compounds in typical cola-flavored carbonated beverages were characterized using gas chromatography-olfactometry and gas chromatography-mass spectrometry. The potent odorants in the top three U.S. brands of regular colas were identified by aroma extract dilution analysis (AEDA). Among the numerous odorants identified, eugenol (spicy, clovelike, sweet) and coumarin (sweet, herbaceous) were predominant in all colas. Other predominant odorants in at least one brand included guaiacol (smoky) and linalool (floral, sweet), while 1,8-cineole (minty, eucalyptus-like) was a moderately potent odorant in all colas. Determination of the enantiomeric compositions indicated that (R)-(-)-linalool (34.5%) was a more potent odorant than the (S)-(+)-enantiomer (65.6%) due to its much lower odor detection threshold. In addition, lemon-lime and cooling attributes determined by sensory descriptive analysis had the highest odor intensities among the eight sensory descriptors. The aroma profiles of the three colas were in good agreement with the potent odorants identified by AEDA.

  4. Characterization of the key aroma compounds in pork soup stock by using an aroma extract dilution analysis. (United States)

    Takakura, Yukiko; Osanai, Hiroki; Masuzawa, Takuya; Wakabayashi, Hidehiko; Nishimura, Toshihide


    The aroma extract dilution analysis of an extract prepared from pork stock and subsequent experiments led to the identification of 15 aroma-active compounds in the flavor dilution factor range of 64-2048. Omission experiments to select the most aroma-active compounds from the 15 odor compounds suggested acetol, octanoic acid, δ-decalactone, and decanoic acid as the main active compounds contributing to the aroma of pork stock. Aroma recombination, addition, and omission experiments of these four aroma compounds in taste-reconstituted pork stock showed that each compound had an individual aroma profile. A comparison of the overall aroma between this recombined mixture and pork stock showed strong similarity, suggesting that the key aroma compounds had been successfully identified.

  5. Characterization of the most aroma-active compounds in cherry tomato by application of the aroma extract dilution analysis. (United States)

    Selli, Serkan; Kelebek, Hasim; Ayseli, Mehmet Turan; Tokbas, Habip


    Aroma and aroma-active compounds of cherry tomato (Lycopersicum esculentum) was analyzed by gas chromatography-mass spectrometry-olfactometry (GC-MS-O). According to sensory analysis, the aromatic extract obtained by liquid-liquid extraction was representative of tomato odour. A total of 49 aroma compounds were identified and quantified in fresh cherry tomato. Aldehydes were qualitatively and quantitatively the most dominant volatiles in cherry tomato, followed by alcohols. Aroma extract dilution analysis (AEDA) was used for the determination of aroma-active compounds of tomato sample. A total of 21 aroma-active compounds were detected in aromatic extract of fresh tomato, of which 18 were identified. On the basis of the flavour dilution (FD) factor, the most powerful aroma-active compounds identified in the extract were (Z)-3-hexenal (FD=1024) and (E)-2-hexenal (FD=256), which were described as the strong green-grassy and green-leafy odour, respectively. The major organic acid and sugar found were citric acid and fructose, respectively.

  6. Comparative Aroma Extract Dilution Analysis (cAEDA) of Fat from Tainted Boars, Castrated Male Pigs, and Female Pigs. (United States)

    Gerlach, Christoph; Leppert, Jan; Santiuste, Alicia Chamarro; Pfeiffer, Anne; Boeker, Peter; Wüst, Matthias


    The aroma profile of porcine fat from tainted boars, female pigs, and castrated male pigs was investigated by application of comparative aroma extract dilution analysis (cAEDA) on a SAFE distillate of volatiles prepared from porcine back fat samples. The AEDA resulted in a total of 16 aroma active compounds for boar fat with flavor dilution (FD) factors ranging from 2 to 2048, whereas 12 aroma active compounds were found in fat of female pigs and 14 in fat of castrated male pigs, both with FD factors ranging from 2 to 32. Odor activity values (OAVs) of key components for each fat were identified: In boar fat androstenone, skatole, indole, and 2-aminoacetophenone showed highest OAVs, whereas 2,5-dimethylpyrazine, 2,4-decadienal, and δ-decalactone showed highest OAVs in fat of female pigs. Fat of castrated male pigs showed highest OAVs for skatole, indole, 1-octen-3-ol and methional. Finally, the off-flavor attributes of boar fat were successfully simulated by a recombinant of all odorants at their natural concentration level in deodorized sunflower oil.

  7. Spectroscopic analysis of hot-water- and dilute-acid-extracted hardwood and softwood chips (United States)

    Lehto, Joni; Louhelainen, Jarmo; Huttunen, Marko; Alén, Raimo


    Hot-water and dilute sulfuric acid pretreatments were performed prior to chemical pulping for silver/white birch (Betula pendula/B. pubescens) and Scots pine (Pinus sylvestris) chips to determine if varying pretreatment conditions on the original wood material were detectable via attenuated total reflectance (ATR) infrared spectroscopy. Pretreatment conditions varied with respect to temperature (130 °C and 150 °C) and treatment time (from 30 min to 120 min). The effects of the pretreatments on the composition of wood chips were determined by ATR infrared spectroscopy. The spectral data were compared to those determined by common wood chemistry analyses to evaluate the suitability of ATR spectroscopy method for rapid detection of changes in the wood chemical composition caused by different pretreatment conditions. In addition to determining wood species-dependent differences in the wood chemical composition, analytical results indicated that most essential lignin- and carbohydrates-related phenomena taking place during hot-water and acidic pretreatments could be described by applying this simple spectral method requiring only a small sample amount and sample preparation. Such information included, for example, the cleavage of essential lignin bonds (i.e., mainly β-O-4 linkages in guaiacyl and syringyl lignin) and formation of newly condensed lignin structures under different pretreatment conditions. Carbohydrate analyses indicated significant removal of hemicelluloses (especially hardwood xylan) and hemicelluloses-derived acetyl groups during the pretreatments, but they also confirmed the highly resistant nature of cellulose towards mild pretreatments.

  8. Comparison of key aroma compounds in five different types of Japanese soy sauces by aroma extract dilution analysis (AEDA). (United States)

    Kaneko, Shu; Kumazawa, Kenji; Nishimura, Osamu


    An investigation by the aroma extract dilution analysis (AEDA) technique of the aroma concentrate from five different types of Japanese soy sauces, categorized according to Japan Agricultural Standards as Koikuchi Shoyu (KS), Usukuchi Shoyu (US), Tamari Shoyu (TS), Sai-Shikomi Shoyu (SSS), and Shiro Shoyu (SS), revealed 25 key aroma compounds. Among them, 3-ethyl-1,2-cyclopentanedione and 2'-aminoacetophenone were identified in the soy sauces for the first time. Whereas 3-(methylthio)propanal (methional) and 3-hydroxy-4,5-dimethyl-2(5H)-furanone (sotolon) were detected in all of the soy sauce aroma concentrates as having high flavor dilution (FD) factors, 4-ethyl-2-methoxyphenol was detected as having a high FD factor in only four of the soy sauces (KS, US, TS, and SSS). Furthermore, 5(or 2)-ethyl-4-hydroxy-2(or 5)-methyl-3(2H)-furanone (4-HEMF) and 4-hydroxy-2,5-dimethyl-3(2H)-furanone (4-HDMF), which were thought to be the key odorants in KS, were detected in KS, US, TS, and SSS, but the FD factors widely varied among them. The sensory evaluations demonstrated that the aroma descriptions of a cooked potato-like note and a caramel-like/seasoning-like note were evaluated as high scores with no significant differences among the five soy sauces. On the other hand, a burnt/spicy note was evaluated as having high scores in KS, TS, and SSS, but it was evaluated as having a low score in SS. The comparative AEDA experiments and the auxiliary sensory experiments demonstrated that the five different types of Japanese soy sauces varied in their key aroma compounds and aroma characteristics, and the key aroma compounds in KS might not always be highly contributing in the other types of Japanese soy sauces.

  9. Characterization of the potent odorants contributing to the characteristic aroma of Chinese green tea infusions by aroma extract dilution analysis. (United States)

    Baba, Ryoko; Kumazawa, Kenji


    The volatile fractions of three famous Chinese green tea cultivar infusions (Longjing, Maofeng, and Biluochun) were prepared by a combination of the adsorptive column method and the SAFE techniques. The aroma extract dilution analysis (AEDA) applied to the volatile fractions revealed 58 odor-active peaks with flavor dilution (FD) factors between 4(1) and 4(7). Forty-six of the odorants, which included six odorants that have not been reported in the literature in Chinese green tea (2-isopropyl-3-methoxypyrazine, 2-ethenyl-3,5-dimethylpyrazine, cis-4,5-epoxy-(E)-2-decenal, 4-ethylguaiacol, (E)-isoeugenol, and 3-phenylpropionic acid), were identified or tentatively identified by GC-MS and GC-O. Among the perceived odorants, 4-hydroxy-2,5-dimethyl-3(2H)-furanone, 3-hydroxy-4,5-dimethyl-2(5H)-furanone, coumarin, vanillin, geraniol, (E)-isoeugenol, and 2-methoxyphenol showed high FD factors in all of the cultivars, irrespective of the cultivar or harvesting season, suggesting that these seven odorants are essential for the aroma of Chinese green tea. On the other hand, the contents of the odorants, FD factors of which were uneven between the cultivars, were suggested to influence the characteristic aroma of each cultivar. In addition, the formation mechanism of (E)-isoeugenol, one of the odorants which have not been reported in the literature with a high FD factor common to all the cultivars, was investigated, and it was suggested that the (E)-isoeugenol content of the tea products has a close correlation with the manufacturing process of the tea leaves.

  10. Aroma extraction dilution analysis of Sauternes wines. Key role of polyfunctional thiols. (United States)

    Bailly, Sabine; Jerkovic, Vesna; Marchand-Brynaert, Jacqueline; Collin, Sonia


    The aim of the present work was to investigate Sauternes wine aromas. In all wine extracts, polyfunctional thiols were revealed to have a huge impact. A very strong bacon-petroleum odor emerged at RI = 845 from a CP-Sil5-CB column. Two thiols proved to participate in this perception: 3-methyl-3-sulfanylbutanal and 2-methylfuran-3-thiol. A strong synergetic effect was evidenced between the two compounds. The former, never mentioned before in wines, and not found in the musts of this study, is most probably synthesized during fermentation. 3-Methylbut-2-ene-1-thiol, 3-sulfanylpropyl acetate, 3-sulfanylhexan-1-ol, and 3-sulfanylheptanal also contribute to the global aromas of Sauternes wines. Among other key odorants, the presence of a varietal aroma (alpha-terpineol), sotolon, fermentation alcohols (3-methylbutan-1-ol and 2-phenylethanol) and esters (ethyl butyrate, ethyl hexanoate, and ethyl isovalerate), carbonyls (trans-non-2-enal and beta-damascenone), and wood flavors (guaiacol, vanillin, eugenol, beta-methyl-gamma-octalactone, and Furaneol) is worth stressing.

  11. Aroma quality assessment of Korean fermented red pepper paste (gochujang) by aroma extract dilution analysis and headspace solid-phase microextraction-gas chromatography-olfactometry. (United States)

    Kang, Kyung-Mo; Baek, Hyung-Hee


    The objective of this study was to assess aroma quality of gochujang using purge and trap, simultaneous steam distillation and solvent extraction (SDE), and headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-olfactometry (GC-O). Nineteen and 28 aroma-active compounds were detected by aroma extract dilution analysis of purge and trap and SDE, respectively. Diallyl disulfide and 3-isobutyl-2-methoxypyrazine played a significant role in the aroma quality of gochujang. Twelve aroma-active compounds were detected by HS-SPME-GC-O based on sample dilution analysis. Methional, diallyl disulfide, and 3-isobutyl-2-methoxypyrazine were the most intense aroma-active compounds. 3-Isobutyl-2-methoxypyrazine was identified for the first time in gochujang.

  12. Verification of key odorants in rose oil by gas chromatography-olfactometry/aroma extract dilution analysis, odour activity value and aroma recombination. (United States)

    Xiao, Zuobing; Li, Jing; Niu, Yunwei; Liu, Qiang; Liu, Junhua


    Rose oil is much too expensive but very popular. It's well known that the flower oil's aroma profile hasn't been intensively investigated. In order to verify the aroma profile of rose oil, the synthetic blend of odorants was prepared and then compared with the original rose oil using electronic nose analysis (ENA) combined with quantitative descriptive analysis (QDA). The odorants from rose oils were screened out by Gas Chromatography-Olfactometry/aroma extract dilution analysis (GC-O/AEDA) combined with odour activity value (OAV). Both ENA and QDA indicated the recombination model derived from OAV and GC-O/AEDA closely resembled the original rose oil. The experiment results show that rose oxide, linalool, α-pinene, β-pinene, nonanal, heptanal citronellal, phenyl ethyl alcohol, benzyl alcohol, eugenol, methyl eugenol, β-citronellol, hexyl acetate, β-ionone, nerol, etc. are very important constituent to rose oil aroma profile.

  13. Characterization of odor-active compounds in sweet-type Chinese rice wine by aroma extract dilution analysis with special emphasis on sotolon. (United States)

    Chen, Shuang; Wang, Dong; Xu, Yan


    The aroma characteristics of sweet-type Chinese rice wine were studied by sensory analysis, aroma extract dilution analysis (AEDA), and quantitative analysis. Sensory evaluation demonstrated that a caramel-like note was the most distinctive characteristic for sweet-type Chinese rice wine. AEDA was carried out on the extract of a typical sweet-type Chinese rice wine sample. Thirty-nine odor-active regions were detected in the sample with a flavor dilution (FD) factor ≥8, and 37 of these were further identified. Among them, sotolon and 2- and 3-methylbutanol showed the highest FD factor of 1024, followed by 2-acetyl-1-pyrroline (tentatively identified), dimethyl trisulfide, 2-phenylethanol, and vanillin with a FD factor of 512. Sotolon was identified as a key aroma compound in Chinese rice wine for the first time. AEDA results indicated that sotolon (caramel-like/seasoning-like) was the potentially key contributor to the caramel-like descriptor of sweet-type Chinese rice wine. The concentration of sotolon in Chinese rice wine was further quantitated by Lichrolut-EN solid-phase extraction coupled with microvial insert large volume injection method. The content of sotolon ranged from 35.93 to 526.17 μg/L, which was above its odor threshold (9 μg/L) for all Chinese rice wine samples. The highest concentration of sotolon was found in the sweet-type Chinese rice wine, which highlighted the important aroma role of sotolon for this particular type of Chinese rice wine.

  14. Characterization of the most odor-active compounds in an American Bourbon whisky by application of the aroma extract dilution analysis. (United States)

    Poisson, Luigi; Schieberle, Peter


    Application of the aroma extract dilution analysis (AEDA) on the volatile fraction carefully isolated from an American Bourbon whisky revealed 45 odor-active areas in the flavor dilution (FD) factor range of 32-4096 among which (E)-beta-damascenone and delta-nonalactone showed the highest FD factors of 4096 and 2048, respectively. With FD factors of 1024, (3S,4S)-cis-whiskylactone, gamma-decalactone, 4-allyl-2-methoxyphenol (eugenol), and 4-hydroxy-3-methoxy-benzaldehyde (vanillin) additionally contributed to the overall vanilla-like, fruity, and smoky aroma note of the spirit. Application of GC-Olfactometry on the headspace above the whisky revealed 23 aroma-active odorants among which 3-methylbutanal, ethanol, and 2-methylbutanal were identified as additional important aroma compounds. Compared to published data on volatile constituents in whisky, besides ranking the whisky odorants on the basis of their odor potency, 13 aroma compounds were newly identified in this study: ethyl (S)-2-methylbutanoate, (E)-2-heptenal, (E,E)-2,4-nonadienal, (E)-2-decenal, (E,E)-2,4-decadienal, 2-isopropyl-3-methoxypyrazine, ethyl phenylacetate, 4-methyl acetophenone, alpha-damascone, 2-phenylethyl propanoate, 3-hydroxy-4,5-dimethyl-2(5H)-furanone, trans-ethyl cinnamate, and (Z)-6-dodeceno-gamma-lactone.

  15. Characterization of Key Aroma Compounds in Raw and Thermally Processed Prawns and Thermally Processed Lobsters by Application of Aroma Extract Dilution Analysis. (United States)

    Mall, Veronika; Schieberle, Peter


    Application of aroma extract dilution analysis (AEDA) to an aroma distillate of blanched prawn meat (Litopenaeus vannamei) (BPM) revealed 40 odorants in the flavor dilution (FD) factor range from 4 to 1024. The highest FD factors were assigned to 2-acetyl-1-pyrroline, 3-(methylthio)propanal, (Z)-1,5-octadien-3-one, trans-4,5-epoxy-(E)-2-decenal, (E)-3-heptenoic acid, and 2-aminoacetophenone. To understand the influence of different processing conditions on odorant formation, fried prawn meat was investigated by means of AEDA in the same way, revealing 31 odorants with FD factors between 4 and 2048. Also, the highest FD factors were determined for 2-acetyl-1-pyrroline, 3-(methylthio)propanal, and (Z)-1,5-octadien-3-one, followed by 4-hydroxy-2,5-dimethyl-3(2H)-furanone, (E)-3-heptenoic acid, and 2-aminoacetophenone. As a source of the typical marine, sea breeze-like odor attribute of the seafood, 2,4,6-tribromoanisole was identified in raw prawn meat as one of the contributors. Additionally, the aroma of blanched prawn meat was compared to that of blanched Norway and American lobster meat, respectively (Nephrops norvegicus and Homarus americanus). Identification experiments revealed the same set of odorants, however, with differing FD factors. In particular, 3-hydroxy-4,5-dimethyl-2(5H)-furanone was found as the key aroma compound in blanched Norway lobster, whereas American lobster contained 3-methylindole with a high FD factor.

  16. Characterization of the key aroma compounds in Turkish olive oils from different geographic origins by application of aroma extract dilution analysis (AEDA). (United States)

    Kesen, Songul; Kelebek, Hasim; Selli, Serkan


    The aroma and aroma-active compounds of olive oils obtained from Nizip Yaglik (NY) and Kilis Yaglik (KY) cultivars and the effect of the geographical area (southern Anatolian and Aegean regions) on these compounds were analyzed by gas chromatography-mass spectrometry-olfactometry (GC-MS-O). For this purpose, two oil samples were obtained from their native geographical area including NY from Nizip province and KY from Kilis province (southern Anatolian region of Turkey). Another two oils of the same cultivar, NY-Bornova (NY-B) and KY-Bornova (KY-B), were obtained from the Olive Oil Research Center-Bornova, Izmir province (Aegean region of Turkey) to compare geographical effect on aroma and aroma-active compounds. Simultaneous distillation and extraction (SDE) with dichloromethane was used for extraction of volatile components. SDE gave a highly representative aromatic extract of the studied olive oil based on the sensory analysis. Totals of 61, 48, 59, and 48 aroma compounds were identified and quantified in olive oils obtained from NY, NY-B, KY, and KY-B cultivars, respectively. The results of principal component analysis (PCA) showed that the aroma profile of native region oils was discriminately different from those of Bornova region oils. Aldehydes and alcohols were qualitatively and quantitatively the most dominant volatiles in the oil samples. Aroma extract dilution analysis (AEDA) was used for the determination of aroma-active compounds of olive oils. The number of aroma-active compounds in native region oils was higher than in Bornova region oils. Within the compounds, aldehydes and alcohols were the largest aroma-active compounds in all olive oils.

  17. Analysis of halogenated and priority pesticides at different concentration levels. Automated SPE extraction followed by isotope dilution-GC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Planas, C.; Saulo, J.; Rivera, J.; Caixach, J. [Institut Investigacions Quimiques i Ambientals (IIQAB-CSIC), Barcelona (Spain)


    In this work, automatic SPE extraction of 16 pesticides and metabolites with the automated Power-Prep trademark system is evaluated at different concentration levels using polymeric (ENV+) and C{sub 18} sorbent phases. The method was optimised by comparing recoveries obtained using different eluting solvents. The optimised procedure was then applied to spiked water samples at concentration levels of 0.1{mu}g/L (quality standard for individual pesticides in drinking water) and 0.02{mu}g/L (close to the detection limit of most pesticides).

  18. Removal of Phenol from Dilute Solutions by Predispersed Solvent Extraction

    Institute of Scientific and Technical Information of China (English)


    Predispersed solvent extraction (PDSE) is a new method for separating solutes from aqueous solution by solvent extraction and one which has shown promise for extraction from extremely dilute solution very efficient and very quick. The use of colloidal liquid aphrons in predispersed solvent extraction may ameliorate the problems such as emulsion formation, reduction of interfacial mass transfer and low interfacial mass transfer areas in solvent extraction process. In present paper, colloidal liquid aphrons are successfully generated using kerosene as a solvent, tributyl phosphate(TBP) as an extractant, sodium dodecyl benzene sulphate(SDBS) as surfactant in aqueous phase and Tween-80 in oil phase. Extraction of phenol from dilute solution was studied by using colloidal liquid aphrons and colloidal gas aphrons in a semi-batch extraction column. It has been found that the PDSE process is more suitable for extraction of dilute solutions. It has also been discovered that the PDSE process has a great advantage over traditional single-stage extraction process.

  19. Application of isotope dilution analysis for the evaluation of extraction conditions in the determination of total selenium and selenomethionine in yeast-based nutritional supplements. (United States)

    Hinojosa Reyes, L; Marchante-Gayón, J M; García Alonso, J I; Sanz-Medel, A


    Isotope dilution analysis (IDA) has been used to quantify total selenium, total solubilized selenium, and the selenomethionine (SeMet) amount in yeast and yeast-based nutritional supplements after acid microwave digestion and different enzymatic extraction procedures. For this purpose, both a (77)Se-enriched SeMet spike, previously synthesized and characterized in our laboratory, and a (77)Se(VI) spike were used. In the analysis of the nutritional supplements, the SeMet spike was added to the sample and extracted under different conditions, and the (78)Se/(77)Se and (80)Se/(77)Se isotope ratios were measured as peak area ratios after high-performance liquid chromatography (HPLC) separation and inductively coupled plasma mass spectrometry (ICP-MS) detection. The formation of SeH(+) and mass discrimination were corrected using a natural SeMet standard injected every three samples. Similarly, total solubilized selenium was measured in the extracts after enzymatic hydrolysis using the (77)Se-enriched SeMet as a spike by direct nebulization without a chromatographic separation. To establish a mass balance, total selenium was also determined by IDA-ICP-MS on the yeast tablets after microwave digestion using (77)Se(VI) as a spike. Results showed that all enzymatic procedures tested were able to solubilize total selenium quantitatively from the solid. However, the recovery for the species SeMet, the major selenium compound detected, was seriously affected by the enzymatic procedure employed and also by the matrix composition of the supplement evaluated. For the yeast sample, SeMet recovery increased from 68 to 76% by the combined use of driselase and protease. For the nutritional supplements, the two most effective procedures appeared to be protease and driselase/protease, with a SeMet recovery ranging from 49 to 63%, depending upon the supplement evaluated. In the case of in vitro gastrointestinal enzymolysis, the results obtained showed 26-37% SeMet recovery, while the

  20. Flux balance analysis accounting for metabolite dilution. (United States)

    Benyamini, Tomer; Folger, Ori; Ruppin, Eytan; Shlomi, Tomer


    Flux balance analysis is a common method for predicting steady-state flux distributions within metabolic networks, accounting for the growth demand for the synthesis of a predefined set of essential biomass precursors. Ignoring the growth demand for the synthesis of intermediate metabolites required for balancing their dilution leads flux balance analysis to false predictions in some cases. Here, we present metabolite dilution flux balance analysis, which addresses this problem, resulting in improved metabolic phenotype predictions.

  1. Quantitative analysis of phosphoric acid esters in aqueous samples by isotope dilution stir-bar sorptive extraction combined with direct analysis in real time (DART)-Orbitrap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bridoux, Maxime C., E-mail: [CEA, DAM, DIF, F-91297 Arpajon (France); Malandain, Hélène [SANTEN SAS, 1 rue Pierre Fontaine, Bâtiment Genavenir IV, F-91058 Evry (France); Leprince, Françoise; Progent, Frédéric; Machuron-Mandard, Xavier [CEA, DAM, DIF, F-91297 Arpajon (France)


    Highlights: • Theory and modeling of organophosphorus SBSE extraction are presented. • Organophosphorus are quantitatively analyzed by isotopic dilution SBSE/DART/Orbitrap-MS. • PDMS coated Twisters™ extract phosphate acid esters in the neutral form from water samples. • Good linearity between concentrations and relative peak areas (0.1–750 ng mL{sup −1}). • This novel SBSE/DART/Orbitrap-MS method should be very valuable for on-site sampling/monitoring - Abstract: A novel hyphenated technique, namely the combination of stir bar sorptive extraction (SBSE) with isotope dilution direct analysis in real time (DART) Orbitrap™ mass spectrometry (OT-MS) is presented for the extraction of phosphoric acid alkyl esters (tri- (TnBP), di- (HDBP), and mono-butyl phosphate (H2MBP)) from aqueous samples. First, SBSE of phosphate esters was performed using a Twister™ coated with 24 μL of polydimethylsiloxane (PDMS) as the extracting phase. SBSE was optimized for extraction pH, phase ratio (PDMS volume/aqueous phase volume), stirring speed, extraction time and temperature. Then, coupling of SBSE to DART/Orbitrap-MS was achieved by placing the Twister™ in the middle of an open-ended glass tube between the DART and the Orbitrap™. The DART mass spectrometric response of phosphate esters was probed using commercially available and synthesized alkyl phosphate ester standards. The positive ion full scan spectra of alkyl phosphate triesters (TnBP) was characterized by the product of self-protonation [M + H]{sup +} and, during collision-induced dissociation (CID), the major fragmentation ions corresponded to consecutive loss of alkyl chains. Negative ionization gave abundant [M − H]{sup −} ions for both HDnBP and H2MnBP. Twisters™ coated with PDMS successfully extracted phosphate acid esters (tri-, di- and mono-esters) granted that the analytes are present in the aqueous solution in the neutral form. SBSE/DART/Orbitrap-MS results show a good linearity between

  2. Characterization of the major aroma-active compounds in mango (Mangifera indica L.) cultivars Haden, White Alfonso, Praya Sowoy, Royal Special, and Malindi by application of a comparative aroma extract dilution analysis. (United States)

    Munafo, John P; Didzbalis, John; Schnell, Raymond J; Schieberle, Peter; Steinhaus, Martin


    The aroma-active compounds present in tree-ripened fruits of the five mango (Mangifera indica L.) cultivars Haden, White Alfonso, Praya Sowoy, Royal Special, and Malindi were isolated by solvent extraction followed by solvent-assisted flavor evaporation (SAFE) and analyzed by gas chromatography-olfactometery (GC-O). Application of a comparative aroma extract dilution analysis (cAEDA) afforded 54 aroma-active compounds in the flavor dilution (FD) factor range from 4 to ≥2048, 16 of which are reported for the first time in mango. The results of the identification experiments in combination with the FD factors revealed 4-hydroxy-2,5-dimethyl-3(2H)-furanone as an important aroma compound in all cultivars analyzed. Twenty-seven aroma-active compounds were present in at least one mango cultivar at an FD factor ≥128. Clear differences in the FD factors of these odorants between each of the mango cultivars suggested that they contributed to the unique sensory profiles of the individual cultivars.

  3. Stable isotope dilution assays in mycotoxin analysis

    Energy Technology Data Exchange (ETDEWEB)

    Rychlik, Michael; Asam, Stefan [Universitaet Muenchen, Lehrstuhl fuer Lebensmittelchemie der Technischen, Garching (Germany)


    The principle and applications of stable isotope dilution assays (SIDAs) in mycotoxin analysis are critically reviewed. The general section includes historical aspects of SIDAs, the prerequisites and limitations of the use of stable isotopically labelled internal standards, and possible calibration procedures. In the application section actual SIDAs for the analysis of trichothecenes, zearalenone, fumonisins, patulin, and ochratoxin A are presented. The syntheses and availability of labelled mycotoxins for use as internal standards is reviewed and specific advances in food analysis and toxicology are demonstrated. The review indicates that LC-MS applications, in particular, require the use of stable isotopically labelled standards to compensate for losses during clean-up and for discrimination due to ion suppression. As the commercial availability of these compounds continues to increase, SIDAs can be expected to find expanding use in mycotoxin analysis. (orig.)

  4. Stable isotope dilution assays in mycotoxin analysis. (United States)

    Rychlik, Michael; Asam, Stefan


    The principle and applications of stable isotope dilution assays (SIDAs) in mycotoxin analysis are critically reviewed. The general section includes historical aspects of SIDAs, the prerequisites and limitations of the use of stable isotopically labelled internal standards, and possible calibration procedures. In the application section actual SIDAs for the analysis of trichothecenes, zearalenone, fumonisins, patulin, and ochratoxin A are presented. The syntheses and availability of labelled mycotoxins for use as internal standards is reviewed and specific advances in food analysis and toxicology are demonstrated. The review indicates that LC-MS applications, in particular, require the use of stable isotopically labelled standards to compensate for losses during clean-up and for discrimination due to ion suppression. As the commercial availability of these compounds continues to increase, SIDAs can be expected to find expanding use in mycotoxin analysis.

  5. Characterization of the Typical Potent Odorants in Chinese Roasted Sesame-like Flavor Type Liquor by Headspace Solid Phase Microextraction-Aroma Extract Dilution Analysis, with Special Emphasis on Sulfur-Containing Odorants. (United States)

    Sha, Sha; Chen, Shuang; Qian, Michael; Wang, Chengcheng; Xu, Yan


    The aroma profile of Chinese roasted sesame-like flavor type liquor was investigated by means of headspace solid phase microextraction-aroma extract dilution analysis (HS-SPME-AEDA). Sixty-three odor-active regions were detected by HS-SPME-AEDA with flavor dilution (FD) factors >5, and 58 of these were further identified. Among them, ethyl hexanoate, 2-furfurylthiol, dimethyl trisulfide, 3-methylbutanal, ethyl butanoate, ethyl 2-methylbutanoate, ethyl pentanoate, and ethyl 4-methylpentanoate appeared with the highest FD factors. In particular, eight sulfur-containing odorants were identified to be potentially important to roasted sesame-like flavor type liquor. The concentration of these odor-active compounds was further quantitated by combination of four different quantitative measurements, and 36 odorants had concentrations higher than their corresponding odor thresholds. On the basis of the odor activity values (OAVs), 2-furfurylthiol (OAV 1182), dimethyl trisulfide (OAV 220), β-damascenone (OAV 116), and methional (OAV 99) could be responsible for the unique aroma of roasted sesame-like flavor type liquor. An aroma recombination model prepared by mixing 36 aroma compounds with OAVs >1 showed a good similarity to the aroma of the original roasted sesame-like flavor type liquor. For the first time, 2-furfurylthiol was determined to be a typical potent odorant in roasted sesame-like flavor type liquor by omission study.

  6. Determination of the stability of diluted allergen extracts using a concentration step prior to EAST inhibition

    NARCIS (Netherlands)

    Niemeijer, NR; Kauffman, HF; DeMonchy, JGR; Meijer, G.


    Background Generally the stability of diluted allergen extracts, as used for skin testing, provocation testing and immunotherapy can not be measured using a normal enzyme allergosorbent test (EAST) inhibition method. Objective The aim of this study was to determine the stability of diluted allergen

  7. Molecular analysis of two mouse dilute locus deletion mutations: Spontaneous dilute lethal20J and radiation-induced dilute prenatal lethal Aa2 alleles

    Energy Technology Data Exchange (ETDEWEB)

    Strobel, M.C.; Seperack, P.K.; Copeland, N.G.; Jenkins, N.A. (National Cancer Institute-Frederick Cancer Research Facility, MD (USA))


    The dilute (d) coat color locus of mouse chromosome 9 has been identified by more than 200 spontaneous and mutagen-induced recessive mutations. With the advent of molecular probes for this locus, the molecular lesion associated with different dilute alleles can be recognized and precisely defined. In this study, two dilute mutations, dilute-lethal20J (dl20J) and dilute prenatal lethal Aa2, have been examined. Using a dilute locus genomic probe in Southern blot analysis, we detected unique restriction fragments in dl20J and Aa2 DNA. Subsequent analysis of these fragments showed that they represented deletion breakpoint fusion fragments. DNA sequence analysis of each mutation-associated deletion breakpoint fusion fragment suggests that both genomic deletions were generated by nonhomologous recombination events. The spontaneous dl20J mutation is caused by an interstitial deletion that removes a single coding exon of the dilute gene. The correlation between this discrete deletion and the expression of all dilute-associated phenotypes in dl20J homozygotes defines the dl20J mutation as a functional null allele of the dilute gene. The radiation-induced Aa2 allele is a multilocus deletion that, by complementation analysis, affects both the dilute locus and the proximal prenatal lethal-3 (pl-3) functional unit. Molecular analysis of the Aa2 deletion breakpoint fusion fragment has provided access to a previously undefined gene proximal to d. Initial characterization of this new gene suggests that it may represent the genetically defined pl-3 functional unit.

  8. An Isotopic Dilution Experiment Using Liquid Scintillation: A Simple Two-System, Two-Phase Analysis. (United States)

    Moehs, Peter J.; Levine, Samuel


    A simple isotonic, dilution analysis whose principles apply to methods of more complex radioanalyses is described. Suitable for clinical and instrumental analysis chemistry students, experimental manipulations are kept to a minimum involving only aqueous extraction before counting. Background information, procedures, and results are discussed.…

  9. Automatic indicator dilution curve extraction in dynamic-contrast enhanced imaging using spectral clustering (United States)

    Saporito, Salvatore; Herold, Ingeborg HF; Houthuizen, Patrick; van den Bosch, Harrie CM; Korsten, Hendrikus HM; van Assen, Hans C.; Mischi, Massimo


    Indicator dilution theory provides a framework for the measurement of several cardiovascular parameters. Recently, dynamic imaging and contrast agents have been proposed to apply the method in a minimally invasive way. However, the use of contrast-enhanced sequences requires the definition of regions of interest (ROIs) in the dynamic image series; a time-consuming and operator dependent task, commonly performed manually. In this work, we propose a method for the automatic extraction of indicator dilution curves, exploiting the time domain correlation between pixels belonging to the same region. Individual time intensity curves were projected into a low dimensional subspace using principal component analysis; subsequently, clustering was performed to identify the different ROIs. The method was assessed on clinically available DCE-MRI and DCE-US recordings, comparing the derived IDCs with those obtained manually. The robustness to noise of the proposed approach was shown on simulated data. The tracer kinetic parameters derived on real images were in agreement with those obtained from manual annotation. The presented method is a clinically useful preprocessing step prior to further ROI-based cardiac quantifications.

  10. Reduction of matrix effects in liquid chromatography-electrospray ionization-mass spectrometry by dilution of the sample extracts: how much dilution is needed? (United States)

    Stahnke, Helen; Kittlaus, Stefan; Kempe, Günther; Alder, Lutz


    In this study, the relationship between matrix concentration and suppression of electrospray ionization (matrix effects) was investigated. Ion suppression of pesticides present in QuEChERS extracts was used as an example. Residue-free extracts of four different commodities, avocado, black tea, orange, and rocket (arugula), were fortified with 39 pesticides each. For many of the resulting 156 pesticide/matrix combinations, considerable matrix effects were observed if the coextracted matrix of 8 mg of equivalent sample (in the case of tea: 1.6 mg) was injected with the undiluted extracts. The reduction of these matrix effects was measured at 10 levels of dilution up to 1000-fold. The results obtained indicate a linear correlation between matrix effects and the logarithm of matrix concentration (or dilution factor) until the zero-effect level of further dilution was reached. Using the logarithmic equations, it could be shown that a dilution of extracts by a factor of 25-40 reduces ion suppression to less than 20% if the initial suppression is ≤80%. For stronger matrix effects or complete elimination of suppression, higher dilution factors were needed. The observed correlation was independent from the two instrument platforms used, but the degree of matrix effects differed slightly between the two mass spectrometers in this study.

  11. Extraction Behaviour of Hexavalent Plutonium in the System of Dilute TBP/Kerosene

    Institute of Scientific and Technical Information of China (English)


    On the basis of the preparation and stabilization of Pu(Ⅵ), the distribution of it between dilute TBP/kerosene and aqueous phase is studied. The influences of the concentration of TBP, HNO3, A1(NO3)3, TBP and UO2(NO3)2 on the extraction of Pu(Ⅵ) by 5%TBP/kerosene are investigated at 28 ℃. The extraction reaction equation, the corresponding apparent equilibrium constant and the free energy change of it at temperature of 28 ℃ are obtained as follows:

  12. Evaluation of method for phthalate extraction from milk related to milk dilution ratio

    Directory of Open Access Journals (Sweden)

    Milojković Danica S.


    Full Text Available Liquid-liquid extraction techniques were compared coupled with gas chromatography-mass spectrometry (GC-MS, for the extraction and the determination of four phthalates: dimethyl phthalate (DMP, di-n-butyl phthalate (DBP, benzyl butyl phthalate (BBP and di-(2-ethylhexyl phthalate (DEHP in six different kinds of milk-based samples. Extraction factors: sample preparation, organic solvent type and volume, salt effect, agitation and the extraction time were optimized. The ion of base peaks (m/z 149 for DBP, BBP and DEHP and m/z 163 for DMP for investigated phthalates were selected for the screening studies. The acquisition was performed at the selected ion monitoring mode. The MSD response for GC-MS phthalate calibration standards was linear between 0.25 and 2.50 μg mL-1 with calculated LODs between 0.01 μg mL-1 to 0.04 μg mL-1 and LOQs of 0.05 μg mL-1 to 0.12 μg mL-1, while repeatability was between 1.7 % to 4.9 % RSD. The study demonstrated an increase of the recovery of less polar phthalates in matrix milk standards by matrix dilution. Recovery for hydrophilic phthalates, like DMP, was not changed by matrix dilution and it was continuously low for the investigated method. Two spiking levels were tested for influence of matrix dilution on phthalate recovery, showed the same trend. [Projekat Ministarstva nauke Republike Srbije, br. 31060

  13. Evaluation of the Single Dilute (0.43 M) Nitric Acid Extraction to Determine Geochemically Reactive Elements in Soil

    NARCIS (Netherlands)

    Groenenberg, Jan E.; Römkens, Paul F.A.M.; Zomeren, van André; Rodrigues, S.M.; Comans, Rob N.J.


    Recently a dilute nitric acid extraction (0.43 M) was adopted by ISO (ISO-17586:2016) as standard for extraction of geochemically reactive elements in soil and soil like materials. Here we evaluate the performance of this extraction for a wide range of elements by mechanistic geochemical modeling

  14. Trace determination of zinc by substoichiometric isotope dilution analysis

    Energy Technology Data Exchange (ETDEWEB)

    Sandhya, D.; Priya, S.; Subramanian, M.O.S. [Indian Institute of Technology, Madras (India)


    A radiometric method based on substoichiometric isotope dilution analysis using 1,10-phenanthroline and a substoichiometric amount of eosin was developed for determining trace amounts of zinc. Evaluation of various metal ion interferences shows that as little as 0.2 {mu}g Zn could be determined in an aqueous-phase volume of 60 mL. The method has been successfully applied to the determination of Zn in city waste incineration ash, cadmium metal, Fourts-B tablets, Boro-plus ointment, and magnesium alloy samples. 12 refs., 3 figs., 3 tabs.

  15. Transient Thermo-Mechanical Analysis of the TPSG4 Beam Diluter

    CERN Document Server

    Goddard, B; Herrera-Martínez, A; Kadi, Y; Marque, S


    A new extraction channel is being built in the Super Proton Synchrotron (SPS) Long Straight Section 4 (LSS4) to transfer proton beams to the Large Hadron Collider (LHC) and also to the CERN Neutrino to Gran Sasso (CNGS) target. The beam is extracted in a fast mode during a single turn. For this purpose a protection of the MSE copper septum coil, in the form of a beam diluting element placed upstream, will be required to cope with the new failure modes associated with the fast extraction operation. The present analysis focuses on the thermo-mechanical behavior of the proposed TPSG4 diluter element irradiated by a fast extracted beam (up to 4.9 x 10^13 protons per 7.2 mus pulse) from the SPS. The deposited energy densities, estimated from primary and secondary particle simulations using the high-energy particle transport code FLUKA, were converted to internal heat generation rates taken as a thermal load input for the finite-element engineering analyses code ANSYS. According to the time dependence of the extrac...

  16. Comparison of key aroma compounds in cooked brown rice varieties based on aroma extract dilution analyses. (United States)

    Jezussek, Magnus; Juliano, Bienvenido O; Schieberle, Peter


    The aroma compounds present in cooked brown rice of the three varieties Improved Malagkit Sungsong (IMS), Basmati 370 (B 370), and Khaskhani (KK), and of the variety Indica (German supermarket sample), were identified on the basis of aroma extract dilution analyses (AEDA). A total of 41 odor-active compounds were identified, of which eleven are reported for the first time as rice constituents. 2-Amino acetophenone (medicinal, phenolic), which was up to now unknown in rice aroma, exhibited the highest flavor dilution (FD) factor among the 30 to 39 odor-active compounds detected in all four varieties. 2-Acetyl-1-pyrroline, exhibiting an intense popcorn-like aroma-note, was confirmed as a further key aroma constituent in IMS, B 370, and KK, but was not important in Indica. Differences in the FD factors between the varieties were found for the previously unknown rice aroma compound 3-hydroxy-4,5-dimethyl-2(5H)-furanone (Sotolon; seasoning-like), which was higher in B 370 than in IMS and KK. In IMS, a yet unknown, spicy smelling component with a very high FD factor could be detected, which contributed with lower FD factors to the overall aromas of B 370 and KK, and was not present in Indica. The latter variety, which was available on the German market, differed most in its overall aroma from the three Asian brown rices.

  17. Dilute alkali and hydrogen peroxide treatment of microwave liquefied rape straw residue for the extraction of cellulose nanocrystals (United States)

    Xingyan Huang; Cornelis F. De Hoop; Feng Li; Jiulong Xie; Chung-Yun Hse; Jinqiu Qi; Yongze Jiang; Yuzhu Chen


    Microwave-assisted liquefaction of rape straw in methanol was conducted to collect the liquefied residues for the extraction of cellulose nanocrystals (CNCs).The liquefied residue with content of 23.44% from 180∘C/7.5 min was used to fibrillate CNCs with dilute alkali (2% NaOH) and hydrogen peroxide (5% H2O2...


    Institute of Scientific and Technical Information of China (English)

    Jian-qiang Chen; Yu-fang Shao; Zhen Yang; Hu Yang; Rong-shi Cheng


    It was found that the interface effects in viscous capillary flow influenced the process of viscosity measurement greatly,and the abnormal viscosity behaviors of polyelectrolytes as well as neutral polymers in dilute solution region were ascribed to interface effect.According to this theory,we have reviewed the previous viscosity data of derivatives of poly-2-vinylpyridine reported by Maclay and Fuoss first.Then,the abnormal viscosity behaviors of a series of sodium polystyrene sulfonate samples with various molecular weights in dilute aqueous solutions were studied further.The solute adsorption behaviors and structural information of polymers have been discussed carefully.

  19. Recovery of Cu(II from diluted aqueous solutions by non-dispersive solvent extraction

    Directory of Open Access Journals (Sweden)

    Alguacil, E. J.


    Full Text Available The removal of copper from diluted aqueous solutions with ACORGA M5640 extractant using non-dispersive solvent extraction technology was studied. It was possible to remove Cu(II below the international standars from solutions having initially as low concentration as 0,01 g/l under various experimental conditions, i.e aqueous pH 4.0, 10 % v/v ACORGA M5640 in Exxol D100, an organic flow of 100 ml/min, and an aqueous flow 50ml/min. Since the removal occurs by chelating ion exchange between copper from solution and protons from the extractant, the former was stripped by using a 180 g/l sulphuric acid solution which flowed (50 ml/min through the tube side organic was passed (400 ml/min through the shell side of the fibers of the module

    Se estudia la eliminación del cobre presente en disoluciones acuosas diluidas empleando el agente de extracción ACORGA M5640 y la tecnología de extracción con disolventes no dispersiva. Bajo las condiciones experimentales estudiadas, pH de la fase acuosa 4,0 ±0,1, 10 % v/v ACORGA M5640 en Exxsol D100, flujo de la fase orgánica 100 ml/min, flujo de la fase acuosa 50 ml/min, es posible eliminar el Cu(II, por debajo de los límites marcados internacionalmente, en disoluciones con un contenido tan bajo como 0,01 g/1 del metal. Debido a que la extracción transcurre mediante un intercambio catiónico (y formación de un compuesto tipo quelato entre el cobre presente en el medio acuoso y los protones del agente de extracción, el metal se puede reextraer mediante la utilización de una disolución de 180 g/1 de ácido sulfúrico que fluye (50 ml/min a través de la parte interior de las fibras del módulo, mientras que la fase orgánica fluye (400 ml/min por la parte exterior de las mismas fibras.

  20. Analysis of boron dilution in a four-loop PWR

    Energy Technology Data Exchange (ETDEWEB)

    Sun, J.G.; Sha, W.T. [Argonne National Lab., IL (United States)


    Thermal mixing and boron dilution in a pressurized water reactor were analyzed with COMMIX codes. The reactor system was the four-loop Zion reactor. Two boron dilution scenarios were analyzed. In the first scenario, the plant is in cold shutdown and the reactor coolant system has just been filled after maintenance on the steam generators. To flush the air out of the steam generator tubes, a reactor coolant pump (RCP) is started, with the water in the pump suction line devoid of boron and at the same temperature as the coolant in the system. In the second scenario, the plant is at hot standby and the reactor coolant system has been heated to operating temperature after a long outage. It is assumed that an RCP is started, with the pump suction line filled with cold unborated water, forcing a slug of diluted coolant down the downcomer and subsequently through the reactor core. The subsequent transient thermal mixing and boron dilution that would occur in the reactor system is simulated for these two scenarios. The reactivity insertion rate and the total reactivity are evaluated and a sensitivity study is performed to assess the accuracy of the numerical modeling of the geometry of the reactor coolant system.

  1. Analysis of boron dilution in a four-loop PWR

    Energy Technology Data Exchange (ETDEWEB)

    Sun, J.G.; Sha, W.T.


    Thermal mixing and boron dilution in a pressurized water reactor were analyzed with COMMIX codes. The reactor system was the four loop Zion reactor. Two boron dilution scenarios were analyzed. In the first scenario, the plant is in cold shutdown and the reactor coolant system has just been filled after maintenance on the steam generators. To flush the air out of the steam generator tubes, a reactor coolant pump (RCP) is started, with the water in the pump suction line devoid of boron and at the same temperature as the coolant in the system. In the second scenario, the plant is at hot standby and the reactor coolant system has been heated up to operating temperature after a long outage. It is assumed that an RCP is started, with the pump suction line filled with cold unborated water, forcing a slug of diluted coolant down the downcomer and subsequently through the reactor core. The subsequent transient thermal mixing and boron dilution that would occur in the reactor system is simulated for these two scenarios. The reactivity insertion rate and the total reactivity are evaluated.

  2. Analysis of ochratoxin A in grapes, musts and wines by LC–MS/MS: First comparison of stable isotope dilution assay and diastereomeric dilution assay methods

    Energy Technology Data Exchange (ETDEWEB)

    Roland, Aurélie, E-mail: [Nyseos, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Bros, Pauline, E-mail: [Institut Français de la Vigne et du Vin, UMT Qualinnov, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Bouisseau, Anaïs, E-mail: [Nyseos, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France); Institut des Biomolécules Max Mousseron, UMR-CNRS-5247, Universités Montpellier I and II, Place Eugène Bataillon, 34095 Montpellier (France); Cavelier, Florine, E-mail: [Institut des Biomolécules Max Mousseron, UMR-CNRS-5247, Universités Montpellier I and II, Place Eugène Bataillon, 34095 Montpellier (France); Schneider, Rémi, E-mail: [Institut Français de la Vigne et du Vin, UMT Qualinnov, 2 place Pierre Viala, Montpellier Cedex 1 34060 (France)


    Highlights: • OTA extraction on immunoaffinity columns is not adapted for DIDA quantification. • The use of a labeled internal standard is compulsory to obtain reliable results. • SIDA and DIDA quantification approaches have been compared for the first time. Abstract: Ochratoxin A (OTA) exhibits potent nephrotoxic, carcinogenic and teratogenic effects and its maximum level in wines has been set to 2 μg L⁻¹ by regulation. Consequently, the analytical procedures for OTA determination in wines have to be both very sensitive and reliable. In this paper, we compared two quantification methods: the stable isotope dilution assay (SIDA) and the diastereomeric dilution assay (DIDA). For this purpose, non-natural analogues of OTA were synthesized: the labeled OTA (OTA-d₄) as a diastereomeric mixture for the SIDA and one non-natural OTA’s diastereomer (OTA-dia) for the DIDA. To quantify OTA in red grapes, musts or wines, the sample preparation was optimized using immunoaffinity column extraction and the analysis was performed by LC–MS/MS in Multiple Reaction Monitoring mode. A validation procedure in agreement with the International Organization of Vine and Wine recommendations was conducted. It appeared that SIDA quantification exhibited excellent sensitivity (LOD < 1 ng L⁻¹), accuracy (recovery = 98%), repeatability (RSD < 3%) and intermediate reproducibility (RSD < 4%) compared to quantification by DIDA. Indeed, DIDA method did not provide satisfactory results demonstrating that immunoaffinity extraction is exclusively selective for the natural OTA and not for its diastereomer, which therefore cannot be considered as a good internal standard for this particular method.

  3. Quantitative Analysis by Isotopic Dilution Using Mass Spectroscopy: The Determination of Caffeine by GC-MS. (United States)

    Hill, Devon W.; And Others


    Describes a laboratory technique for quantitative analysis of caffeine by an isotopic dilution method for coupled gas chromatography-mass spectroscopy. Discusses caffeine analysis and experimental methodology. Lists sample caffeine concentrations found in common products. (MVL)

  4. Effects of diluting medium and holding time on sperm motility analysis by CASA in ram. (United States)

    Mostafapor, Somayeh; Farrokhi Ardebili, Farhad


    The aim of this study was to evaluate the effects of dilution rate and holding time on various motility parameters using computer-assisted sperm analysis (CASA). The semen samples were collected from three Ghezel rams. Samples were diluted in seminal plasma (SP), phosphate-buffered saline (PBS) containing 1% bovine serum albumin (BSA) and Bioexcell. The motility parameters that computed and recorded by CASA include curvilinear velocity (VCL), straight line velocity (VSL), average path velocity (VAP), straightness (STR), linearity (LIN), amplitude of lateral head displacement (ALH), and beat cross frequency (BCF). In all diluters, there was a decrease in the average of all three parameters of sperms movement velocity as the time passed, but density of this decrease was more intensive in SP. The average of ALH between diluters indicated a significant difference, as it was more in Bioexcell in comparison with the similar amount in SP and PBS. The average of LIN in the diluted sperms in Bioexcell was less than two other diluters in all three times. The motility parameters of the diluted sperms in Bioexcell and PBS indicated an important and considerable difference with the diluted sperms in SP. According to the gained results, the Bioexcell has greater ability in preserving motility of sperm in comparison with the other diluters but as SP is considered as physiological environment for sperm. It seems that the evaluation of the motility parameters in Bioexcell and PBS cannot be an accurate and comparable evaluation with SP.

  5. Enhancement of enzymatic saccharification of corn stover with sequential Fenton pretreatment and dilute NaOH extraction. (United States)

    He, Yu-Cai; Ding, Yun; Xue, Yu-Feng; Yang, Bin; Liu, Feng; Wang, Cheng; Zhu, Zheng-Zhong; Qing, Qing; Wu, Hao; Zhu, Cheng; Tao, Zhi-Cheng; Zhang, Dan-Ping


    In this study, an effective method by the sequential Fenton pretreatment and dilute NaOH extraction (FT-AE) was chosen for pretreating corn stover. Before dilute NaOH (0.75 wt%) extraction at 90 °C for 1h, Fenton reagent (0.95 g/L of FeSO4 and 29.8 g/L of H2O2) was employed to pretreat CS at a solid/liquid ratio of 1/20 (w/w) at 35 °C for 30 min. The changes in the cellulose structural characteristics (porosity, morphology, and crystallinity) of the pretreated solid residue were correlated with the enhancement of enzymatic saccharification. After being enzymatically hydrolyzed for 72 h, the reducing sugars and glucose from the hydrolysis of 60 g/L FT-AE-CS pretreated could be obtained at 40.96 and 23.61 g/L, respectively. Finally, the recovered hydrolyzates containing glucose had no inhibitory effects on the ethanol fermenting microorganism. In conclusion, the sequential Fenton pretreatment and dilute NaOH extraction has high potential application in future.

  6. Extraction of beryllium from refractory beryllium oxide with dilute ammonium bifluoride and determination by fluorescence: a multiparameter performance evaluation. (United States)

    Goldcamp, Michael J; Goldcamp, Diane M; Ashley, Kevin; Fernback, Joseph E; Agrawal, Anoop; Millson, Mark; Marlow, David; Harrison, Kenneth


    Beryllium exposure can cause a number of deleterious health effects, including beryllium sensitization and the potentially fatal chronic beryllium disease. Efficient methods for monitoring beryllium contamination in workplaces are valuable to help prevent dangerous exposures to this element. In this work, performance data on the extraction of beryllium from various size fractions of high-fired beryllium oxide (BeO) particles (from Beryllium concentrations were determined by fluorescence using a hydroxybenzoquinoline fluorophore. The effects of ABF concentration and volume, extraction temperature, sample tube types, and presence of filter or wipe media were examined. Three percent ABF extracts beryllium nearly twice as quickly as 1% ABF; extraction solution volume has minimal influence. Elevated temperatures increase the rate of extraction dramatically compared with room temperature extraction. Sample tubes with constricted tips yield poor extraction rates owing to the inability of the extraction medium to access the undissolved particles. The relative rates of extraction of Be from BeO of varying particle sizes were examined. Beryllium from BeO particles in fractions ranging from less than 32 microm up to 212 microm were subjected to various extraction schemes. The smallest BeO particles are extracted more quickly than the largest particles, although at 90 degrees C even the largest BeO particles reach nearly quantitative extraction within 4 hr in 3% ABF. Extraction from mixed cellulosic-ester filters, cellulosic surface-sampling filters, wetted cellulosic dust wipes, and cotton gloves yielded 90% or greater recoveries. Scanning electron microscopy of BeO particles, including partially dissolved particles, shows that dissolution in dilute ABF occurs not just on the exterior surface but also via accessing particles' interiors due to porosity of the BeO material. Comparison of dissolution kinetics data shows that as particle diameter approximately doubles, extraction

  7. Online determination of copper in aluminum alloy by microchip solvent extraction using isotope dilution ICP-MS method. (United States)

    Kagawa, Tsuyoshi; Ohno, Masashi; Seki, Tatsuya; Chikama, Katsumi


    Isotope dilution mass spectroscopy (IDMS)/ICP-MS combined with microchip solvent extraction was successfully applied for the online determination of copper in an aluminum alloy. The microchip solvent extraction was developed for the separation of Cu from major element, and optimal pH range was wider than that of the batchwise extraction method. The dimensions of the microchip were 30 mm x 70 mm and that of micro-channel on the microchip was 180 microm wide and 40 microm deep. The copper complex with 8-hydroxyquinoline was extracted into o-xylene at pH 5.5 and back extracted with 0.1 mol l(-1) nitric acid at flow rate of 20 microl min(-1). The total extraction efficiency (water/organic solvent/nitric acid) was around 40%. IDMS/ICP-MS was coupled with solvent extraction for precise determination of Cu. The extraction and back-extraction on the microchip took about 1s and the total measurement time for the IDMS/ICP-MS was about 40s/sample. The blank value of this method was 0.1 ng g(-1). The proposed method was used for the determination of Cu in Al standard materials (JSAC 0121-C, The Japan Society for Analytical Chemistry and 7074 Al alloy, Nippon Light Metal Co. Ltd.). The obtained analytical results are in good agreement with the certified values.

  8. Recovery of Pu,Np in 1BP of Dilute TBP Extraction Process

    Institute of Scientific and Technical Information of China (English)


    <正>In the TBP extraction process, Np and Pu need to be recovered from effluents of the TBP extraction process. In this work, the recovery of Np and Pu from TBP extraction effluents is studied was investigated

  9. Separation of Indium and Iron from Dilute Sulphate Solutions with a Phosphorous Mixer Extractant

    Institute of Scientific and Technical Information of China (English)


    The phosphorous mixer introduced could replace D2EHPA as an extractant applied in the extraction of indium. The extraction properties of the phosphorous mixer were studied. The influences of extractant concentration, organic/aqueous (O/A) phase ratio, equilibrium time, and pH value of the feed solutions on the extraction of indium and separation of indium-iron were investigated experimentally. Under the best operating conditions, more than 98% of indium was extracted through two-stage counter-current extraction. The optimizing condition of indium extraction is determined as follows: O/A = 1∶(9€?2) in volume ratio; 30% PPD in sulphonated kerosene; pH of the feed, about 0.6; equilibrium time, 3€? min. The extractant has good reusing and anti-aging properties.

  10. Effect of wine dilution on the reliability of tannin analysis by protein precipitation

    DEFF Research Database (Denmark)

    Jensen, Jacob Skibsted; Werge, Hans Henrik Malmborg; Egebo, Max


    A reported analytical method for tannin quantification relies on selective precipitation of tannins with bovine serum albumin. The reliability of tannin analysis by protein precipitation on wines having variable tannin levels was evaluated by measuring the tannin concentration of various dilutions...... of five commercial red wines. Tannin concentrations of both very diluted and concentrated samples were systematically underestimated, which could be explained by a precipitation threshold and insufficient protein for precipitation, respectively. Based on these findings, we have defined a valid range...

  11. Computational Analysis of Intersubject Variability and Thrombin Generation in Dilutional Coagulopathy (United States)


    T R A N S F U S I O N P R A C T I C E Computational analysis of intersubject variability and thrombin generation in dilutional coagulopathy_3610 2475... intersubject variability. STUDY DESIGN AND METHODS: A thoroughly vali- dated computational model was used to simulate throm- bin generation curves for 472...parameters in diluted blood plasma displayed significant intersubject variabil- ity (with a coefficient of variation up to approx. 28%). Nevertheless

  12. Antiphospholipid syndrome: analysis of dilute Russell's viper venom time titer. (United States)

    Martinez, Alan P; Cunningham, Mark T


    To evaluate the characteristic features of the dilute Russell's viper venom time (DRVVT) titer in the antiphospholipid syndrome (APS). The medical record of 3660 consecutive patients with DRVVT orders between 2006 and 2015 were examined for criteria satisfying the diagnosis of APS. DRVVT titer was studied as a function of titer distribution, titer stability, and clinicopathologic features. Twenty-six patients were diagnosed with APS based on a persistently positive DRVVT and a history of arterial or venous thrombosis. DRVVT titer was mostly of low magnitude (65-77% of patients), was of similar value between initial and repeat testing (mean DRVVT titer 1.40 vs. 1.38; P = 0.858; mean time interval 216 days), and was positively associated with anticardiolipin antibodies (IgG and IgM) and antibeta-2-glycoprotein I antibodies (IgG and IgM) (P antiphospholipid antibody profile in 0 and 62% of patients, respectively (P antiphospholipid antibody profiles.

  13. Stable isotope dilution analysis of hydrologic samples by inductively coupled plasma mass spectrometry (United States)

    Garbarino, J.R.; Taylor, H.E.


    Inductively coupled plasma mass spectrometry is employed in the determination of Ni, Cu, Sr, Cd, Ba, Ti, and Pb in nonsaline, natural water samples by stable isotope dilution analysis. Hydrologic samples were directly analyzed without any unusual pretreatment. Interference effects related to overlapping isobars, formation of metal oxide and multiply charged ions, and matrix composition were identified and suitable methods of correction evaluated. A comparability study snowed that single-element isotope dilution analysis was only marginally better than sequential multielement isotope dilution analysis. Accuracy and precision of the single-element method were determined on the basis of results obtained for standard reference materials. The instrumental technique was shown to be ideally suited for programs associated with certification of standard reference materials.

  14. Extraction and analysis of indole derivatives from fungal biomass. (United States)

    Gartz, J


    The occurrence and extraction of indole derivatives in six species from four genera of higher fungi were investigated. By using pure methanol for extraction of the mushrooms analysis revealed the highest concentrations of psilocybin and baeocystin. The psilocin content of the species was higher by using aqueous solutions of alcohols than with methanol alone but was an artificial phenomenon caused by enzymatic destruction of psilocybin. The extraction with dilute acetic acid yielded better results than with the water containing alcohols. The simple one-step procedure with methanol for the quantitative extraction is still the safest method to obtain the genuine alkaloids from fungal biomass.

  15. Optimization and validation of a taste dilution analysis to characterize wine taste. (United States)

    Lopez, R; Mateo-Vivaracho, L; Cacho, J; Ferreira, V


    A procedure for the general taste dilution analysis (TDA) of wine has been optimized and applied to characterize the tastants of 5 different wines. Samples are concentrated first by vacuum distillation at 20 degrees C to obtain a dearomatized concentrate. Such concentrate is redissolved in water and injected in a semipreparative C18-high performance liquid chromatography (HPLC) column. The effluent is separated in fractions that are collected and concentrated by vacuum distillation. Sequential dilutions of the fractions are further evaluated by a sensory panel to assess the intensity of the basic tastes and in-mouth sensations. Fractions were also submitted to HPLC-mass spectrometry (MS) analysis to screen for known tastants of wines. The Taste Dilution chromatograms showed that taste differences between wines are mainly located in fractions 1, 2, and 6, and are mainly related to bitterness and astringency. Different aspects of the method setup and of its reliability are evaluated and discussed.

  16. Mercury speciation analysis in seafood by species-specific isotope dilution: method validation and occurrence data

    Energy Technology Data Exchange (ETDEWEB)

    Clemens, Stephanie; Guerin, Thierry [Agence Nationale de Securite Sanitaire de l' Alimentation, Laboratoire de Securite des Aliments de Maisons-Alfort, Unite des Contaminants Inorganiques et Mineraux de l' Environnement, ANSES, Maisons-Alfort (France); Monperrus, Mathilde; Donard, Olivier F.X.; Amouroux, David [IPREM UMR 5254 CNRS - Universite de Pau et des Pays de l' Adour, Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, Institut des Sciences Analytiques et de Physico-chimie pour l' Environnement et les Materiaux, Pau Cedex (France)


    Methylmercury (MeHg) and total mercury (THg) in seafood were determined using species-specific isotope dilution analysis and gas chromatography combined with inductively coupled plasma mass spectrometry. Sample preparation methods (extraction and derivation step) were evaluated on certified reference materials using isotopically enriched Hg species. Solid-liquid extraction, derivation by propylation and automated agitation gave excellent accuracy and precision results. Satisfactory figures of merit for the selected method were obtained in terms of limit of quantification (1.2 {mu}g Hg kg{sup -1} for MeHg and 1.4 {mu}g Hg kg{sup -1} for THg), repeatability (1.3-1.7%), intermediate precision reproducibility (1.5% for MeHg and 2.2% for THg) and trueness (bias error less than 7%). By means of a recent strategy based on accuracy profiles ({beta}-expectation tolerance intervals), the selected method was successfully validated in the range of approximately 0.15-5.1 mg kg{sup -1} for MeHg and 0.27-5.2 mg kg{sup -1} for THg. Probability {beta} was set to 95% and the acceptability limits to {+-}15%. The method was then applied to 62 seafood samples representative of consumption in the French population. The MeHg concentrations were generally low (1.9-588 {mu}g kg{sup -1}), and the percentage of MeHg varied from 28% to 98% in shellfish and from 84% to 97% in fish. For all real samples tested, methylation and demethylation reactions were not significant, except in one oyster sample. The method presented here could be used for monitoring food contamination by MeHg and inorganic Hg in the future to more accurately assess human exposure. (orig.)

  17. Antioxidant activity of aqueous extract of noni in dilutent for ram semen cryopreservation

    Directory of Open Access Journals (Sweden)

    Ana Lauren Costa Nascimento


    Full Text Available Noni (Morinda citrifolia L. is a fruit consumed worldwide because of its nutritional and therapeutic properties resulting from the large amount of phenolic compounds, which has aroused interest of the scientific community. In order to identify new natural sources of antioxidants, the objective of this study was to evaluate the performance of noni in diluent for ram semen cryopreservation. A completely randomized design consisting of four treatments and three repetitions per treatment was used. The treatments differed in terms of the concentration of the aqueous extract of noni added to the diluent: control, no addition of the extract, and three concentrations (24, 72, and 120 µg/mL. The physical and chemical variables of the mature fruit were evaluated: total acidity (8.78, pH (4.12, and soluble solids (8.18%. The vitamin C content was 309.42 mg per 100 g fresh matter. The aqueous extract of noni was also evaluated regarding the quantity of total phenolic compounds, antioxidant activity, and lipid peroxidation inhibition capacity. The aqueous extract contained a moderate amount of phenolic compounds (47.96 ± 1.95 mg gallic acid equivalent/100 g extract. The concentrations of the aqueous extract of 72 and 120 µg/mL in diluent used for semen cryopreservation inhibited lipid peroxidation by 21.75% and 51.32%, respectively. There was no positive effect of the lowest concentration (24 µg/mL. The antioxidant activity index of noni was 33.33, corresponding to very strong antioxidant activity. The aqueous extract of noni exhibits very strong antioxidant activity and its addition to the diluent for semen cryopreservation at a concentration of 72 µg/mL is able to inhibit lipid peroxidation.

  18. Use of image analysis for monitoring the dilution of Physalis peruviana pulp

    Directory of Open Access Journals (Sweden)

    Silvana Licodiedoff


    Full Text Available The aim of this work was to develop linear models using the image analysis coupled with density measurements to monitor the dilution of the Physalis juice in the concentrations ranging from 0 to 100% in mass of juice pulp. A sample corresponding to 20% in the mass of juice pulp was for validating purposes and a prediction of 19.9±0.3%. The models with three parameters showed the best predictions, providing this technique with a promising future for the monitoring the dilution of fruit juices.

  19. Isotopic Dilution Analysis and Secular Equilibrium Study: Two Complementary Radiochemistry Experiments. (United States)

    Williams, Kathryn R.; Lipford, Levin C.


    Describes a complementary pair of radiochemistry experiments for instruction of isotopic dilution analysis and secular equilibrium. Both experiments use the readily available cesium-137 nuclide and the simple precipitation technique for cesium with the tetraphenylborate anion. Procedures used and typical results obtained are provided and…

  20. A comparison of an optimised sequential extraction procedure and dilute acid leaching of elements in anoxic sediments, including the effects of oxidation on sediment metal partitioning. (United States)

    Larner, Bronwyn L; Palmer, Anne S; Seen, Andrew J; Townsend, Ashley T


    The effect of oxidation of anoxic sediment upon the extraction of 13 elements (Cd, Sn, Sb, Pb, Al, Cr, Mn, Fe, Co, Ni, Cu, Zn, As) using the optimised Community Bureau of Reference of the European Commission (BCR) sequential extraction procedure and a dilute acid partial extraction procedure (4h, 1 molL(-1) HCl) was investigated. Elements commonly associated with the sulfidic phase, Cd, Cu, Pb, Zn and Fe exhibited the most significant changes under the BCR sequential extraction procedure. Cd, Cu, Zn, and to a lesser extent Pb, were redistributed into the weak acid extractable fraction upon oxidation of the anoxic sediment and Fe was redistributed into the reducible fraction as expected, but an increase was also observed in the residual Fe. For the HCl partial extraction, sediments with moderate acid volatile sulfide (AVS) levels (1-100 micromolg(-1)) showed no significant difference in element partitioning following oxidation, whilst sediments containing high AVS levels (>100 micromolg(-1)) were significantly different with elevated concentrations of Cu and Sn noted in the partial extract following oxidation of the sediment. Comparison of the labile metals released using the BCR sequential extraction procedure (SigmaSteps 1-3) to labile metals extracted using the dilute HCl partial extraction showed that no method was consistently more aggressive than the other, with the HCl partial extraction extracting more Sn and Sb from the anoxic sediment than the BCR procedure, whilst the BCR procedure extracted more Cr, Co, Cu and As than the HCl extraction.

  1. Relationship between total concentration and dilute HCl extraction of heavy metals in sediments of harbors and coastal areas in Korea. (United States)

    Choi, Ki Young; Kim, Suk Hyun; Chon, Hyo Taek


    Total concentrations of Cr, Ni, Cu, Zn, Cd and Pb in surface sediments were determined to investigate the regional trends of heavy metal contamination in 11 coastal areas in Korea. Enrichment factor (EF) of heavy metals was calculated by comparing the level of their regional background. The averages of EF values in study areas were 0.99 for Cr, 1.05 for Ni, 4.23 for Cu, 1.80 for Zn, 3.92 for Cd and 1.54 for Pb, respectively. Dilute HCl extractions were useful to deduce the anthropogenic sources of heavy metals and the 1 M HCl extractable fractions of each metal varied from 0.3 to 37.3% for Cr, 1.9 to 66.3% for Ni, 4.2 to 92.9% for Cu, 7.1 to 99.7% for Zn, 10.9 to 98.9% for Cd and 15.0 to 99.1% for Pb. Comparing 1 M HCl extractable fraction to total concentration, large portions of Cu, Zn, Cd and Pb were present as potentially bioavailable fractions from anthropogenic input and were significantly correlated with their EF values showing r > 0.68.

  2. Determination of Trace Cadmium in Geological Samples by Aerosol Dilution ICP-MS with Inverse Aqua Regia Extraction (United States)

    Xu, Q.; Guo, W.; Jin, L.; Hu, S.; Chai, X.


    Cadmium (Cd) is a trace element that occurs at ppb level in most terrestrial materials. The determination of Cd in geological samples by ICP-MS is subject to Zr and/or Mo based oxide/hydroxide interference. This study developed a valid method for the determination of Cd by Ar aerosol dilution ICP-MS with inverse aqua regia extraction (in a water bath at 95℃ for 2h). An Agilent 7700x ICP-MS (Agilent Technologies, USA) with an aerosol dilution system was used. The extraction procedure separated most of the Zr matrix (>90%) from the analyte, and the residual Zr- hydroxides and Mo-oxides or hydroxides were successfully eliminated by adding an amount of Ar to the sample aerosol prior to the plasma. Compared to the conventional operation, the amounts of oxide and hydroxide ions formed in the plasma were reduced by up to 10 times. The relative yields of the interfering oxides and hydroxides were as low as 0.012% ((94Mo16OH++95Mo16O+)/(94Mo++95Mo+)) and 0.007% (94Zr16OH+/94Zr+). Under the optimized dilution gas flow rate (0.85 L min-1) and carrier gas flow rate (0.24 L min-1), the limit of detection (LOD, 3s) for 111Cd was 1.3 ng g-1. The accuracy of the method was assessed by using two USGS SRMs (andesite AGV-2 and basalt BCR-2). The Cd contents determined for AGV-2 and BCR-2 are 0.058±0.004μg g-1 and 0.148±0.007μg g-1 (N=10), which are in good agreement with the USGS reference values (0.061μg g-1 and 0.14μg g-1). The proposed method was also applied to determine Cd contents in 65 IGGE SRMs (28 soils, 28 sediments and 9 rocks). The measured Cd levels in these samples agree well with their certified values. The developed method shows great potential for the direct determination of trace levels of Cd in geological samples.

  3. Analysis of Cyanide in Blood by Headspace-Isotope-Dilution-GC-MS

    DEFF Research Database (Denmark)

    Løbger, Lise Lotte; Petersen, Henning Willads; Andersen, Jens Enevold Thaulov


    An uncomplicated, rapid, automated procedure for the analysis of low cyanide concentrations in whole blood is reported. The analysis was performed by headspace gas chromatography and mass spectrometry in the (1H12C14N) and m/z 29 (1H13C15N). Carryover from cyanide adsorption onto the surface...... of the needle was prevented by developing a new method that enabled automated flushing of the needle in between each cyanide analysis. Results were compared of ordinary calibrations and those of isotope dilutions. The total time of analysis was 18min for a single cyanide analysis....

  4. Brewing Bokashi: Strengthening Student Skills in Dilution Theory through Fermentation Analysis

    Directory of Open Access Journals (Sweden)

    Robert E. Zdor


    Full Text Available One of the basic microbiological techniques that students should master is that of using dilution theory to calculate the levels of bacteria in a fluid. This tip reports on using a rice water-milk fermentation mixture termed Bokashi as an easily implemented exercise in the basic microbiological lab to give students multiple opportunities to use dilution theory. Due to the shifts in bacterial community composition over time, a variety of microbes can be cultured using selective and nonselective media. Microscopic observation and the use of GEN III microplates to determine the collective phenotypic pattern of the mixture both give additional opportunities for students to hone their skills in bacterial analysis. Due to the decrease in the pH of the mixture over time, the notion of acid tolerance in bacteria can be explored and assessed using the microplate. By performing multiple rounds of serial dilutions and spread plating, students can practice their skill at using dilution theory several times over the course of the exercise.

  5. Analysis of heterogeneous boron dilution transients during outages with APROS 3D nodal core model

    Energy Technology Data Exchange (ETDEWEB)

    Kuopanportti, Jaakko [Fortum Power and Heat Ltd, Nuclear Production, Fortum (Finland)


    A diluted water plug can form inside the primary coolant circuit if the coolant flow has stopped at least temporarily. The source of the clean water can be external or the fresh water can build up internally during boiling/condensing heat transfer mode, which can occur if the primary coolant inventory has decreased enough during an accident. If the flow restarts in the stagnant primary loop, the diluted water plug can enter the reactor core. During outages after the fresh fuel has been loaded and the temperature of the coolant is low, the dilution potential is the highest because the critical boron concentration is at the maximum. This paper examines the behaviour of the core as clean or diluted water plugs of different sizes enter the core during outages. The analysis were performed with the APROS 3D nodal core model of Loviisa VVER-440, which contains an own flow channel and 10 axial nodes for each fuel assembly. The widerange cross section data was calculated with CASMO-4E. According to the results, the core can withstand even large pure water plugs without fuel failures on natural circulation. The analyses emphasize the importance of the simulation of the backflows inside the core when the reactor is on natural circulation.

  6. Application of 2D-HPLC/taste dilution analysis on taste compounds in aniseed (Pimpinella anisum L.). (United States)

    Pickrahn, Stephen; Sebald, Karin; Hofmann, Thomas


    This is the first application of fully automated, preparative, two-dimensional HPLC combined with sensory analysis for taste compound discovery using a sweet and licorice-like bitter-tasting aniseed extract as an example. Compared to the traditional iterative fractionation of food extracts by sensory-guided sequential application of separation techniques, the fully automated 2D-HPLC allowed the comprehensive separation of the aniseed extract into 256 subfractions and reduced the fractionation time from about 1 week to <1day. Using a smart sensory strategy to locate high-impact fractions, e.g., by evaluating first-dimension fractions by reconstituting them from second-dimension subfractions, followed by straightforward application of the taste dilution analysis on the individual second-dimension subfractions revealed the sweet-tasting trans-anethole and the bitter-tasting trans-pseudoisoeugenol 2-methylbutyrate, showing recognition thresholds of 70 and 68 μmol/L, respectively, as the primary orosensory active compounds in aniseed. 2D-HPLC combined with smart sensory analysis seems to be a promising strategy to speed the discovery of the key players imparting the attractive taste of foods.

  7. Simultaneous analysis of folic acid and pantothenic acid in foods enriched with vitamins by stable isotope dilution assays

    Energy Technology Data Exchange (ETDEWEB)

    Rychlik, Michael


    Folic and pantothenic acid were quantified in multivitamin products by stable isotope dilution assays using [{sup 2}H{sub 4}]folic acid and [{sup 13}C{sub 3},{sup 15}N]pantothenic acid as the internal standards. Detection was achieved by liquid chromatography/mass spectrometry which enabled unequivocal determination of the vitamins. Due to the very simple extraction procedure, analysis of the vitamins was completed within 2 h. When analyzing multivitamin sweets, the intra-assay and inter-assay coefficient of variation was 3.2% (n=5) and 3.1% (n=5) for folic acid and 4.5% (n=5) as well as 6.5% (n=7) for pantothenic acid, respectively. Along with the precision data, recovery values of 99.4% for folic acid and 103% for pantothenic acid at addition levels of 6 mg/kg and 600 {mu}g/kg, respectively, to starch products proved the accuracy of the new method. Application of the stable isotope dilution assay to fruit juices, whey products, cereals, sweets, pharmaceuticals, wheat flour and salt fortified with one or both vitamins revealed that for the majority of products the labeled pantothenic acid contents were exceeded by about 30%, whereas for folic acid also significantly lower contents than the label claim were found.

  8. Statistical analysis of data from dilution assays with censored correlated counts. (United States)

    Quiroz, Jorge; Wilson, Jeffrey R; Roychoudhury, Satrajit


    Frequently, count data obtained from dilution assays are subject to an upper detection limit, and as such, data obtained from these assays are usually censored. Also, counts from the same subject at different dilution levels are correlated. Ignoring the censoring and the correlation may provide unreliable and misleading results. Therefore, any meaningful data modeling requires that the censoring and the correlation be simultaneously addressed. Such comprehensive approaches of modeling censoring and correlation are not widely used in the analysis of dilution assays data. Traditionally, these data are analyzed using a general linear model on a logarithmic-transformed average count per subject. However, this traditional approach ignores the between-subject variability and risks, providing inconsistent results and unreliable conclusions. In this paper, we propose the use of a censored negative binomial model with normal random effects to analyze such data. This model addresses, in addition to the censoring and the correlation, any overdispersion that may be present in count data. The model is shown to be widely accessible through the use of several modern statistical software. Copyright © 2012 John Wiley & Sons, Ltd.

  9. [Determination of nine hazardous elements in textiles by inductively coupled plasma optical emission spectrometer after microwave-assisted dilute nitric acid extraction]. (United States)

    Chen, Fei; Xu, Dian-dou; Tang, Xiao-ping; Cao, Jing; Liu, Ya-ting; Deng, Jian


    Textiles are easily contaminated by heavy metals in the course of processing. In order to monitor the quality of textiles, a new method was developed for simultaneous determination of arsenic, antimony, lead, cadmium, chromium, cobalt, copper, nickel and mercury in textiles by inductively coupled plasma optical emission spectrometry (ICP-OES) after microwave-assisted dilute nitric acid extraction. After optimizing extraction conditions, we ultimately selected 5% nitric acid as extractant and 5 min as extraction time with the extraction temperature of 120 degrees C and instrument power of 400W in the microwave-assisted extraction procedure. Nine hazardous elements were detected sequentially by ICP-OES. The results showed that the detection limits were 0.3-15 microg x L(-1) and the recoveries 73.6%-105% with the RSDs (n = 3) of 0.1%-3%. The proposed method was successfully used to determine nine elements in cotton, wool, terylene and acrylic.

  10. The Aperture and Layout of the LHC Extraction Septa and TCDS Diluter with an Enlarged MSDC Vacuum Chamber

    CERN Document Server

    Goddard, B


    The LHC beam dumping system must safely abort the LHC beams over the whole energy range, under all realistically possible fault conditions. These include normal operation, failure of machine elements and also abnormal performance of subsystems of the beam dumping system itself. To avoid unnecessary irradiation and even equipment damage, the MSD extraction septa must provide sufficient aperture both for the circulating and extracted beams. In order to satisfy this requirement, a modified (enlarged) vacuum chamber design will be used for the limiting MSDC septa. The analysis of the available apertures is presented, with emphasis on the dependence on the local orbit and beam emittance.

  11. Determination of closantel and rafoxanide in animal tissues by online anionic mixed-mode solid-phase extraction followed by isotope dilution liquid chromatography tandem mass spectrometry. (United States)

    Lai, Shirley Sau Ling; Yeung, Hoi Sze; Lee, Wai On; Ho, Clare; Wong, Yiu Tung


    A rapid and high-throughput isotope dilution LC-MS/MS method with online sample pre-concentration and clean-up using anionic mixed-mode SPE was described for the determination of closantel and rafoxanide in edible bovine and ovine tissues. Tissue samples were extracted with acetonitrile and acetone mixture (60:40, v/v). Sample pre-concentration, clean-up and analysis were completed simultaneously with the online MAX SPE LC-MS/MS system. Closantel-(13) C(6) and rafoxanide-(13) C(6) were used as the internal standards to improve the precision of the method. The method was validated with edible ovine and bovine tissues (muscle, kidney and liver) fortified at three different levels. The accuracy and RSD were 86-106% and ≤14%, respectively. This high-throughput method was suitable for routine quantitative analysis of closantel and rafoxanide in food safety surveillance samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Stable Isotope Dilution Analysis of Gibberellin Residues in Tomato Paste by Liquid Chromatography-Tandem Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    SUN Li; ZHAO Yan-sheng; NIE Xue-mei; LING Yun; CHU Xiao-gang; SHANG De-jun; DONG Ying


    An accurate and sensitive method for the simultaneous determination of gibberellic acid(GA3),gibberellin A4(GA4) and gibberellin A7(GA7) residues in tomato paste was developed by coupling solid phase extraction to high performance liquid chromatography-tandem mass spectrometry(LC-MS/MS) with electrospray ionization based stable isotope dilution analysis(SIDA).The isotope labeled internal standard can compensate for the losses during the extraction and cleanup steps and for discrimination due to ion suppression.After extraction from methanol,hydrophile lipophilic balance(HLB) solid phase extraction(SPE) column was tested for the capacity of the cleanup of the tomato paste in compared with C18 SPE column which is the common way to the detection of GAs,and the former gained better result.Spiked experiments were performed in the non-contaminated tomato pastes and the recoveries of GA3,GA4 and GA7 were 42.6%-75.0% in external standard method(ESM) and 91.1%-103.8% in internal standard method(ISM) respectively.The validities of this method were investigated and good analytical performance for the three GAs was obtained,including low limits of method detection(2 ng/g for GA3 and GA4,0.3 ng/g for GA7),excellent linear dynamic ranges(5-500 ng/g for GA3 and GA4,1-100 ng/g for GAy) and good relative standard deviation ranges(4.8%-9.4% for the intra-day test and 3.5%-11.9% for the inter-day test).

  13. Quantification of fentanyl in serum by isotope dilution analysis using capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan); Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki


    The quantitative determination of fentanyl (FT) in serum was examined by isotope dilution analysis using a capillary gas chromatograph equipped with a surface ionization detector. The separation of FT and its deuterated analogue, FT-{sup 2}H{sub 19}, was achieved within 15 min a column temperature of 260degC by using a 25 m column. Measurement of the samples prepared by the addition of a known amount of FT in the range of 0.2 to 40 ng/ml with 20 ng/ml of FT-{sup 2}H{sub 19} to human control serum allowed observation of a linear relationship between the peak area ratio and the added amount ratio. The correlation coefficient obtained by regression analysis was 0.999. The advantage of the present isotope dilution method was demonstrated by comparison with other FT analogues which substituted a propionyl group with an acetyl group or a phenethyl group with a benzyl group as the internal standard. The present method was used to determine the serum level of FT in surgical patients after i.v. administration. No endogenous compounds and concomitant drugs interfered with the detection of FT or FT-{sup 2}H{sub 19}. This method was considered to be useful for the pharmacokinetic study of FT in patients. (author)

  14. Inorganic and Radiochemical Analysis of AW-101 and AN-107 ''Diluted Feed'' Materials

    Energy Technology Data Exchange (ETDEWEB)

    MW Urie; JJ Wagner; LR Greenwood; OT Farmer; SK Fiskum; RT Ratner; CZ Soderquist


    This report presents the inorganic and radiochemical analytical results for AW-101 and AN-107 diluted feed materials. The analyses were conducted in support of the BNFL Proposal No. 29952/29953 Task 2.1. The inorganic and radiochemical analysis results obtained from the diluted feed materials are used to provide initial characterization information for subsequent processing testing. Quality Assurance (QA) Plan MCS-033 provides the operational and quality control protocols for the analytical activities.

  15. The effect of dilution and the use of a post-extraction nucleic acid purification column on the accuracy, precision, and inhibition of environmental DNA samples (United States)

    Mckee, Anna M.; Spear, Stephen F.; Pierson, Todd W.


    Isolation of environmental DNA (eDNA) is an increasingly common method for detecting presence and assessing relative abundance of rare or elusive species in aquatic systems via the isolation of DNA from environmental samples and the amplification of species-specific sequences using quantitative PCR (qPCR). Co-extracted substances that inhibit qPCR can lead to inaccurate results and subsequent misinterpretation about a species’ status in the tested system. We tested three treatments (5-fold and 10-fold dilutions, and spin-column purification) for reducing qPCR inhibition from 21 partially and fully inhibited eDNA samples collected from coastal plain wetlands and mountain headwater streams in the southeastern USA. All treatments reduced the concentration of DNA in the samples. However, column purified samples retained the greatest sensitivity. For stream samples, all three treatments effectively reduced qPCR inhibition. However, for wetland samples, the 5-fold dilution was less effective than other treatments. Quantitative PCR results for column purified samples were more precise than the 5-fold and 10-fold dilutions by 2.2× and 3.7×, respectively. Column purified samples consistently underestimated qPCR-based DNA concentrations by approximately 25%, whereas the directional bias in qPCR-based DNA concentration estimates differed between stream and wetland samples for both dilution treatments. While the directional bias of qPCR-based DNA concentration estimates differed among treatments and locations, the magnitude of inaccuracy did not. Our results suggest that 10-fold dilution and column purification effectively reduce qPCR inhibition in mountain headwater stream and coastal plain wetland eDNA samples, and if applied to all samples in a study, column purification may provide the most accurate relative qPCR-based DNA concentrations estimates while retaining the greatest assay sensitivity.

  16. [Butanol extraction combined with dilute hydrochloric acid dissolution-atomic fluorescence spectrometric method for indirect determination of molybdenum in Chinese herbal medicine]. (United States)

    Lu, Jian-Ping; Geng, Guo-Xing; Tang, Yan-Kui; Lu, Zhi-Yong


    A method for indirectly determining the molybdenum in Chinese herbal medicine by butanol extraction and dilute hydrochloric acid dissolution was established for atomic fluorescence spectrometry. The molybdoarsenate heteropoly acid, formed in the presence of As(V) and ammonium molybdate in 0.3 mol x L(-1) sulphuric acid medium, was separated and enriched in the organic solvent, then the evaporation of organic reagent was implemented and the left residue was dissolved in dilute hydrochloric acid in which the arsenic content was determined on behalf of molybdenum. In the optimum experimental conditions, molybdenum content in 0-15 microg x L(-1) range depicts a good linear relationship, the detection limit and relative standard deviation of 0.44 microg x L(-1) and 1.1% were obtained, respectively. Spiked Chinese herbal medicine samples were determined with the proposed method, and recoveries of 95.6%-101.3% were achieved.

  17. Quantitative gas chromatography-olfactometry carried out at different dilutions of an extract. Key differences in the odor profiles of four high-quality Spanish aged red wines. (United States)

    Ferreira, V; Aznar, M; López, R; Cacho, J


    Four Spanish aged red wines made in different wine-making areas have been extracted, and the extracts and their 1:5, 1:50, and 1:500 dilutions have been analyzed by a gas chromatography-olfactometry (GC-O) approach in which three judges evaluated odor intensity on a four-point scale. Sixty-nine different odor regions were detected in the GC-O profiles of wines, 63 of which could be identified. GC-O data have been processed to calculate averaged flavor dilution factors (FD). Different ANOVA strategies have been further applied on FD and on intensity data to check for significant differences among wines and to assess the effects of dilution and the judge. Data show that FD and the average intensity of the odorants are strongly correlated (r(2) = 0.892). However, the measurement of intensity represents a quantitative advantage in terms of detecting differences. For some odorants, dilution exerts a critical role in the detection of differences. Significant differences among wines have been found in 30 of the 69 odorants detected in the experiment. Most of these differences are introduced by grape compounds such as methyl benzoate and terpenols, by compounds released by the wood, such as furfural, (Z)-whiskey lactone, Furaneol, 4-propylguaiacol, eugenol, 4-ethylphenol, 2,6-dimethoxyphenol, isoeugenol, and ethyl vanillate, by compounds formed by lactic acid bacteria, such as 2,3-butanedione and acetoine, or by compounds formed during the oxidative storage of wines, such as methional, sotolon, o-aminoacetophenone, and phenylacetic acid. The most important differences from a quantitative point of view are due to 2-methyl-3-mercaptofuran, 4-propylguaiacol, 2,6-dimethoxyphenol, and isoeugenol.

  18. Simple and accurate measurement of carbamazepine in surface water by use of porous membrane-protected micro-solid-phase extraction coupled with isotope dilution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Teo, Hui Ling [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore); Wong, Lingkai [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Liu, Qinde, E-mail: [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Teo, Tang Lin; Lee, Tong Kooi [Chemical Metrology Division, Applied Sciences Group, Health Sciences Authority, 1 Science Park Road, #01-05/06, The Capricorn, Singapore Science Park II, Singapore 117528 (Singapore); Lee, Hian Kee, E-mail: [Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543 (Singapore)


    To achieve fast and accurate analysis of carbamazepine in surface water, we developed a novel porous membrane-protected micro-solid-phase extraction (μ-SPE) method, followed by liquid chromatography-isotope dilution tandem mass spectrometry (LC-IDMS/MS) analysis. The μ-SPE device (∼0.8 × 1 cm) was fabricated by heat-sealing edges of a polypropylene membrane sheet to devise a bag enclosing the sorbent. The analytes (both carbamazepine and isotope-labelled carbamazepine) were first extracted by μ-SPE device in the sample (10 mL) via agitation, then desorbed in an organic solvent (1 mL) via ultrasonication. Several parameters such as organic solvent for pre-conditioning of μ-SPE device, amount of sorbent, adsorption time, and desorption solvent and time were investigated to optimize the μ-SPE efficiency. The optimized method has limits of detection and quantitation estimated to be 0.5 ng L{sup −1} and 1.6 ng L{sup −1}, respectively. Surface water samples spiked with different amounts of carbamazepine (close to 20, 500, and 1600 ng L{sup −1}, respectively) were analysed for the validation of method precision and accuracy. Good precision was obtained as demonstrated by relative standard deviations of 0.7% for the samples with concentrations of 500 and 1600 ng kg{sup −1}, and 5.8% for the sample with concentration of 20 ng kg{sup −1}. Good accuracy was also demonstrated by the relative recoveries in the range of 96.7%–103.5% for all samples with uncertainties of 1.1%–5.4%. Owing to the same chemical properties of carbamazepine and isotope-labelled carbamazepine, the isotope ratio in the μ-SPE procedure was accurately controlled. The use of μ-SPE coupled with IDMS analysis significantly facilitated the fast and accurate measurement of carbamazepine in surface water. - Highlights: • μ-SPE coupled with IDMS for the measurement of carbamazepine. • The method is the first report of coupling μ-SPE with IDMS. • μ-SPE is fast, time

  19. Studies on accuracy of trichothecene multitoxin analysis using stable isotope dilution assays. (United States)

    Asam, S; Rychlik, M


    Critical parameters in mycotoxin analysis were examined by using stable isotope-labelled tricho-thecenes. Sample weight was downsized to 1 g without loosing precision when sufficiently homogenized samples were taken for analysis. Complete extraction of trichothecenes could be achieved with a solvent mixture of acetonitrile+water (84+16; v+v) even without the use of stable isotope labelled standards. However, in particular for the analysis of deoxynivalenol the absolute amount of water in the solvent volume used for extraction appeared critical. Depending on the matrix a low water amount resulted in too low quantitative values when no stable isotope-labelled standards are applied to correct for incomplete extraction. In this case the used extraction volume had to be at least 10 ml for 1 g sample when acetonitrile + water (84+16; v+v) was used as extraction solvent.Losses during sample preparation using two different clean-up columns were not observed. On the contrary, matrix suppression in the ESI-interface of the LC-MS equipment was found to be a serious problem. Depending on the matrix, the latter effect resulted in considerably lower values for trichothecenes when no stable isotope-labelled standards were used to counterbalance this suppression.

  20. Surface lignin change pertaining to the integrated process of dilute acid pre-extraction and mechanical refining of poplar wood chips and its impact on enzymatic hydrolysis. (United States)

    Liu, Wei; Chen, Wei; Hou, Qingxi; Zhang, Jinping; Wang, Bing


    Dilute acid pre-extraction enhanced the mechanically refined poplar pulp substrates' enzymatic hydrolysis efficiency obviously. The results showed that the surface lignin distribution was changed significantly in residual wood chips and pulp substrates, and the surface lignin distribution showed important impact on the following enzymatic hydrolysis. Acid pre-extraction can lead to a redistribution of lignin in fiber cell walls, i.e., the lignin was degraded and migrated to fiber surface in the form of re-deposited lignin and pseudo-lignin. However, higher pre-extraction intensity was not desired due to the formation of redeposited lignin and pseudo-lignin. This study will help to reach a deeper understanding on the lignin distribution in the view of molecular and ultrastructure, and promote the development of a cost-efficient pretreatment strategy for biomass processing.

  1. New Data on Joint Extraction of Nitric Acid, Uranium(VI) and Tetravalent Elements by Diluted TBP and New Approach to Modeling of their Distribution

    Energy Technology Data Exchange (ETDEWEB)

    Zilberman, B.Ya.; Fedorov, Yu.S.; Puzikov, E.A.; Blazheva, I.V. [RPA ' V.G. Khlopin Radium Institute' , 28, 2nd Murinskiy av., Saint-Petersburg, 194021 (Russian Federation)


    HNO{sub 3} and U(IV) extraction by diluted TBP (tributyl phosphate) appeared significantly higher than believed earlier, requiring correction of mathematical model for extraction of all the species. The proposed model of HNO{sub 3} extraction includes its dissolving in the extracted water, as well as its abduction to UO{sub 2}(NO{sub 3}){sub 2}(TBP){sub 2}. Extraction of U(VI) and tetravalent elements is considered as reaction of their hydrated or partially hydrolyzed forms, the latter could be extracted themselves or as neutral forms with water liberation. The equation of element chemical reaction for modeling is determined by the slope of the linear part of the S-shaped curve representing D/S{sup 2} function as a plot of HNO{sub 3} concentration, where D is a distribution coefficient of the micro-component and S is a TBP concentration free of HNO{sub 3}. The description of tetravalent element extraction in U(VI) presence needs the assumption of cation-cation interaction of element hydrolyzed forms with U(VI) in aqueous phase. Zr distribution is affected by micellar effects. (authors)

  2. Evaluation of matrix effect in isotope dilution mass spectrometry based on quantitative analysis of chloramphenicol residues in milk powder

    Energy Technology Data Exchange (ETDEWEB)

    Li, Xiu Qin; Yang, Zong; Zhang, Qing He, E-mail:; Li, Hong Mei


    Graphical abstract: -- Highlights: •We develop a strategy to evaluate matrix effect and its impact on the IDMS results. •Matrix effect and IDMS correction factor from different conditions are evaluated. •Ion suppression effect is observed in LLE and HLB pre-treated sample solutions. •Ion enhancement effect is found in MCX pre-treated sample solution. •IDMS correction factor in HLB and MCX solutions in three instruments is close to 1 -- Abstract: In the present study, we developed a comprehensive strategy to evaluate matrix effect (ME) and its impact on the results of isotope dilution mass spectrometry (IDMS) in analysis of chloramphenicol (CAP) residues in milk powder. Stable isotope-labeled internal standards do not always compensate ME, which brings the variation of the ratio (the peak area of analyte/the peak area of isotope). In our investigation, impact factors of this variation were studied in the extraction solution of milk powder using three mass spectrometers coupled with different ion source designs, and deuterium-labeled chloramphenicol (D5-CAP) was used as the internal standard. ME from mobile phases, sample solvents, pre-treatment methods, sample origins and instruments was evaluated, and its impact on the results of IDMS was assessed using the IDMS correction factor (θ). Our data showed that the impact of ME of mobile phase on the correction factor was significantly greater than that of sample solvent. Significant ion suppression and enhancement effects were observed in different pre-treated sample solutions. The IDMS correction factor in liquid–liquid extraction (LLE) and molecular imprinted polymer (MIP) extract with different instruments was greater or less 1.0, and the IDMS correction factor in hydrophilic lipophilic balance (HLB) and mix-mode cation exchange (MCX) extract with different instruments was all close to 1.0. To the instrument coupled with different ion source design, the impact of ME on IDMS quantitative results was

  3. Doping control analysis of 46 polar drugs in horse plasma and urine using a 'dilute-and-shoot' ultra high performance liquid chromatography-high resolution mass spectrometry approach. (United States)

    Kwok, Wai Him; Choi, Timmy L S; Kwok, Karen Y; Chan, George H M; Wong, Jenny K Y; Wan, Terence S M


    The high sensitivity of ultra high performance liquid chromatography coupled with high resolution mass spectrometry (UHPLC-HRMS) allows the identification of many prohibited substances without pre-concentration, leading to the development of simple and fast 'dilute-and-shoot' methods for doping control for human and equine sports. While the detection of polar drugs in plasma and urine is difficult using liquid-liquid or solid-phase extraction as these substances are poorly extracted, the 'dilute-and-shoot' approach is plausible. This paper describes a 'dilute-and-shoot' UHPLC-HRMS screening method to detect 46 polar drugs in equine urine and plasma, including some angiotensin-converting enzyme (ACE) inhibitors, sympathomimetics, anti-epileptics, hemostatics, the new doping agent 5-aminoimidazole-4-carboxamide-1-β-d-ribofuranoside (AICAR), as well as two threshold substances, namely dimethyl sulfoxide and theobromine. For plasma, the sample (200μL) was protein precipitated using trichloroacetic acid, and the resulting supernatant was diluted using Buffer A with an overall dilution factor of 3. For urine, the sample (20μL) was simply diluted 50-fold with Buffer A. The diluted plasma or urine sample was then analysed using a UHPLC-HRMS system in full-scan ESI mode. The assay was validated for qualitative identification purpose. This straightforward and reliable approach carried out in combination with other screening procedures has increased the efficiency of doping control analysis in the laboratory. Moreover, since the UHPLC-HRMS data were acquired in full-scan mode, the method could theoretically accommodate an unlimited number of existing and new doping agents, and would allow a retrospectively search for drugs that have not been targeted at the time of analysis.

  4. Measurement of isotope abundance variations in nature by gravimetric spiking isotope dilution analysis (GS-IDA). (United States)

    Chew, Gina; Walczyk, Thomas


    Subtle variations in the isotopic composition of elements carry unique information about physical and chemical processes in nature and are now exploited widely in diverse areas of research. Reliable measurement of natural isotope abundance variations is among the biggest challenges in inorganic mass spectrometry as they are highly sensitive to methodological bias. For decades, double spiking of the sample with a mix of two stable isotopes has been considered the reference technique for measuring such variations both by multicollector-inductively coupled plasma mass spectrometry (MC-ICPMS) and multicollector-thermal ionization mass spectrometry (MC-TIMS). However, this technique can only be applied to elements having at least four stable isotopes. Here we present a novel approach that requires measurement of three isotope signals only and which is more robust than the conventional double spiking technique. This became possible by gravimetric mixing of the sample with an isotopic spike in different proportions and by applying principles of isotope dilution for data analysis (GS-IDA). The potential and principle use of the technique is demonstrated for Mg in human urine using MC-TIMS for isotopic analysis. Mg is an element inaccessible to double spiking methods as it consists of three stable isotopes only and shows great potential for metabolically induced isotope effects waiting to be explored.

  5. Soluble/insoluble (dilute-HCl-extractable fractionation of Cd, Pb and Cu in Antarctic snow and its relationship with metal fractionations in the aerosol

    Directory of Open Access Journals (Sweden)

    Annibaldi A.


    Full Text Available A chemical fractionation methodology for determination of the (water soluble and the insoluble (dilute-HCl-extractable fractions of Cd, Pb and Cu in Antarctic snow was set-up and verified for the additivity of the two fractions detected. Molten samples were filtrated and the water-insoluble fraction was extracted by dilute ultrapure HCl (pH ~1.5. Metal determinations were carried out in the two fractions by square wave anodic stripping voltammetry. The total metal concentrations in samples collected in the 2000–2001 austral summer in a clean area (Faraglione Camp in the neighbourhood of the Mario Zucchelli Italian Station were of the order of Cd 10-20 pg g−1, Pb 20–40 pg g−1, Cu 60–120 pg g−1 with an approximate equidistribution between soluble and insoluble fractions. These fractionations compare well (and show a quite consistent temporal trend with those observed in the aerosol samples collected in the same area/period and confirm the close relationship between metal distributions in snow/ice and in the aerosol. At the station metal concentrations increase due to anthropic contribution and the distribution changes with Cd predominantly present in the soluble fraction (~80%, while Pb and Cu are more concentrated in the insoluble fraction, 70–80% and ~70%, respectively.

  6. Determination of low methylmercury concentrations in peat soil samples by isotope dilution GC-ICP-MS using distillation and solvent extraction methods. (United States)

    Pietilä, Heidi; Perämäki, Paavo; Piispanen, Juha; Starr, Mike; Nieminen, Tiina; Kantola, Marjatta; Ukonmaanaho, Liisa


    Most often, only total mercury concentrations in soil samples are determined in environmental studies. However, the determination of extremely toxic methylmercury (MeHg) in addition to the total mercury is critical to understand the biogeochemistry of mercury in the environment. In this study, N2-assisted distillation and acidic KBr/CuSO4 solvent extraction methods were applied to isolate MeHg from wet peat soil samples collected from boreal forest catchments. Determination of MeHg was performed using a purge and trap GC-ICP-MS technique with a species-specific isotope dilution quantification. Distillation is known to be more prone to artificial MeHg formation compared to solvent extraction which may result in the erroneous MeHg results, especially with samples containing high amounts of inorganic mercury. However, methylation of inorganic mercury during the distillation step had no effect on the reliability of the final MeHg results when natural peat soil samples were distilled. MeHg concentrations determined in peat soil samples after distillation were compared to those determined after the solvent extraction method. MeHg concentrations in peat soil samples varied from 0.8 to 18 μg kg(-1) (dry weight) and the results obtained with the two different methods did not differ significantly (p=0.05). The distillation method with an isotope dilution GC-ICP-MS was shown to be a reliable method for the determination of low MeHg concentrations in unpolluted soil samples. Furthermore, the distillation method is solvent-free and less time-consuming and labor-intensive when compared to the solvent extraction method. Copyright © 2014 Elsevier Ltd. All rights reserved.

  7. Brewing Bokashi: Strengthening Student Skills in Dilution Theory through Fermentation Analysis

    National Research Council Canada - National Science Library

    Zdor, Robert E


    .... This tip reports on using a rice water-milk fermentation mixture termed Bokashi as an easily implemented exercise in the basic microbiological lab to give students multiple opportunities to use dilution theory...

  8. Statistical analysis of data from limiting dilution cloning to assess monoclonality in generating manufacturing cell lines. (United States)

    Quiroz, Jorge; Tsao, Yung-Shyeng


    Assurance of monoclonality of recombinant cell lines is a critical issue to gain regulatory approval in biological license application (BLA). Some of the requirements of regulatory agencies are the use of proper documentations and appropriate statistical analysis to demonstrate monoclonality. In some cases, one round may be sufficient to demonstrate monoclonality. In this article, we propose the use of confidence intervals for assessing monoclonality for limiting dilution cloning in the generation of recombinant manufacturing cell lines based on a single round. The use of confidence intervals instead of point estimates allow practitioners to account for the uncertainty present in the data when assessing whether an estimated level of monoclonality is consistent with regulatory requirements. In other cases, one round may not be sufficient and two consecutive rounds are required to assess monoclonality. When two consecutive subclonings are required, we improved the present methodology by reducing the infinite series proposed by Coller and Coller (Hybridoma 1983;2:91-96) to a simpler series. The proposed simpler series provides more accurate and reliable results. It also reduces the level of computation and can be easily implemented in any spreadsheet program like Microsoft Excel. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:1061-1068, 2016.

  9. Pushing the detection limit of infrared spectroscopy for structural analysis of dilute protein samples. (United States)

    Baldassarre, Maurizio; Barth, Andreas


    Fourier-transform infrared spectroscopy is a powerful and versatile tool to investigate the structure and dynamics of proteins in solution. The intrinsically low extinction coefficient of the amide I mode, the main structure-related oscillator, together with the high infrared absorptivity of aqueous media, requires that proteins are studied at high concentrations (>10 mg L(-1)). This may represent a challenge in the study of aggregation-prone proteins and peptides, and questions the significance of structural data obtained for proteins physiologically existing at much lower concentrations. Here we describe the development of a simple experimental approach that increases the detection limit of protein structure analysis by infrared spectroscopy. Our approach relies on custom-made filters to isolate the amide I region (1700-1600 cm(-1)) from irrelevant spectral regions. The sensitivity of the instrument is then increased by background attenuation, an approach consisting in the use of a neutral density filter, such as a non-scattering metal grid, to attentuate the intensity of the background spectrum. When the filters and grid are combined, a 2.4-fold improvement in the noise level can be obtained. We have successfully tested this approach using a highly diluted solution of pyruvate kinase in deuterated medium (0.2% w/v), and found that it provides spectra of a quality comparable to those recorded with a 10-fold higher protein concentration.

  10. Analysis of polonium-210 in food products and bioassay samples by isotope-dilution alpha spectrometry. (United States)

    Lin, Zhichao; Wu, Zhongyu


    A rapid and reliable radiochemical method coupled with a simple and compact plating apparatus was developed, validated, and applied for the analysis of (210)Po in variety of food products and bioassay samples. The method performance characteristics, including accuracy, precision, robustness, and specificity, were evaluated along with a detailed measurement uncertainty analysis. With high Po recovery, improved energy resolution, and effective removal of interfering elements by chromatographic extraction, the overall method accuracy was determined to be better than 5% with measurement precision of 10%, at 95% confidence level.

  11. Characterisation of the dilute HCl extraction method for the identification of metal contamination in Antarctic marine sediments. (United States)

    Snape, I; Scouller, R C; Stark, S C; Stark, J; Riddle, M J; Gore, D B


    A regional survey of potential contaminants in marine or estuarine sediments is often one of the first steps in a post-disturbance environmental impact assessment. Of the many different chemical extraction or digestion procedures that have been proposed to quantify metal contamination, partial acid extractions are probably the best overall compromise between selectivity, sensitivity, precision, cost and expediency. The extent to which measured metal concentrations relate to the anthropogenic fraction that is bioavailable is contentious, but is one of the desired outcomes of an assessment or prediction of biological impact. As part of a regional survey of metal contamination associated with Australia's past waste management activities in Antarctica, we wanted to identify an acid type and extraction protocol that would allow a reasonable definition of the anthropogenic bioavailable fraction for a large number of samples. From a kinetic study of the 1 M HCl extraction of two Certified Reference Materials (MESS-2 and PACS-2) and two Antarctic marine sediments, we concluded that a 4 h extraction time allows the equilibrium dissolution of relatively labile metal contaminants, but does not favour the extraction of natural geogenic metals. In a regional survey of 88 marine samples from the Casey Station area of East Antarctica, the 4 h extraction procedure correlated best with biological data, and most clearly identified those sediments thought to be contaminated by runoff from abandoned waste disposal sites. Most importantly the 4 h extraction provided better definition of the low to moderately contaminated locations by picking up small differences in anthropogenic metal concentrations. For the purposes of inter-regional comparison, we recommend a 4 h 1 M HCl acid extraction as a standard method for assessing metal contamination in Antarctica.

  12. Extraction and elemental analysis of Coleus forskohlii extract

    Directory of Open Access Journals (Sweden)

    Haritha Kanne


    Full Text Available Background: Coleus forskohlii Willd. is a popular traditional medicine used since ancient times for treatment of heart diseases, abdominal colic and respiratory disorders. Objective: The aim of this study was to characterize the root extract of the medicinal plant Coleus forskohlii. Materials and Methods: Dry roots of C. forskohlii were used to extract Forskolin using toluene as a solvent. Thus, obtained extract of C. forskohlii was standardized to 30% and used for further studies. Results: The physical properties of the extract were analyzed through scanning electron microscopy analysis, while the characterization of root extract through X-ray diffraction (XRD and element analysis. The morphological feature of the C. forskohlii extract showed a flake like structure and the XRD showed sulfur trioxide (SO 3 and trimer of sulfur trioxide (S 3 O 9 . Through element analysis, elements such as carbon, oxygen, magnesium, aluminum, silicon, phosphorous, and sulfur were identified. Carbon showed the highest weight of 75.49% in comparison to all other elements.

  13. Diglycolic acid modified zirconium phosphate and studies on the extraction of Am(III) and Eu(III) from dilute nitric acid medium

    Energy Technology Data Exchange (ETDEWEB)

    Selvan, B. Robert; Suneesh, A.S.; Venkatesan, K.A.; Antony, M.P. [Indira Gandhi Centre for Atomic Research, Kalpakkam (India). Fuel Chemistry Division; Dasthaiah, K.; Gardas, R.L. [Indian Institute of Technology - Madras, Chennai (India). Dept. of Chemistry


    Diglycolic acid modified zirconium phosphate (ZrP-DGA) was prepared and studied for the extraction of Am(III) and Eu(III) from dilute nitric acid medium. The distribution coefficient (K{sub d}, mL.g{sup -1}) of Am(III) and Eu(III) was measured as a function of time, pH and concentration of Eu(III) ion etc. The K{sub d} of Am(III) and Eu(III) increased with increase of pH, reached a maximum value of distribution coefficient at pH 1.5 - 2, followed by decrease in K{sub d} values. Rapid extraction of Am(III) and Eu(III) in ZrP-DGA was observed followed by the establishment of equilibrium occurred in 100 min. Kinetics of extraction was fitted in to pseudo second order rate equation. The amount of Eu(III) loaded in ZrP-DGA increased with increase in the concentration of Eu(III) ion in aqueous phase and the isotherm was fitted in to Langmuir and Freundlich adsorption models. The extraction of Am(III) in ZrP-DGA was higher as compared to Eu(III) and the interference of Eu(III) on the extraction of Am(III) was studied. The distribution coefficient of some lanthanides in ZrP-DGA was measured and the K{sub d} of lanthanides increased across the lanthanide series. The extracted trivalent metal ions were recovered in three contacts of loaded ZrP-DGA with 0.5 M nitric acid.

  14. Mixotrophic growth and biochemical analysis of Chlorella vulgaris cultivated with diluted monosodium glutamate wastewater. (United States)

    Ji, Yan; Hu, Wenrong; Li, Xiuqing; Ma, Guixia; Song, Mingming; Pei, Haiyan


    Monosodium glutamate wastewater (MSGW) is a potential medium for microbial cultivation because of containing abundant organic nutrient. This paper seeks to evaluate the feasibility of growing Chlorella vulgaris with MSGW and assess the influence of MSGW concentration on the biomass productivity and biochemical compositions. The MSGW diluted in different concentrations was prepared for microalga cultivation. C. vulgaris growth was greatly promoted with MSGW compared with the inorganic BG11 medium. C. vulgaris obtained the maximum biomass concentration (1.02 g/L) and biomass productivity (61.47 mg/Ld) with 100-time diluted MSGW. The harvested biomass was rich in protein (36.01-50.64%) and low in lipid (13.47-25.4%) and carbohydrate (8.94-20.1%). The protein nutritional quality and unsaturated fatty acids content of algal increased significantly with diluted MSGW. These results indicated that the MSGW is a feasible alternative for mass cultivation of C. vulgaris.

  15. Reaction product analysis of aconitine in dilute ethanol using ESI-Q-ToF-MS. (United States)

    Tan, Peng; Liu, Yong-Gang; Li, Fei; Qiao, Yan-Jiang


    The study was done to identify the reaction products of aconitine in dilute ethanol using electrospray ionization-triple quad time-of-flight mass spectrometry (ESI-Q-TOF-MS). Five hydrolysates were detected, their pseudo-molecules are 632, 604, 586, 570, 500, they are 8-ethyoxyl-14-benzoylaconitine, benzoylaconine, pyraconitine, 8-acetyl-14-ethyoxylaconitine, aconine, respectively. Among them, 8-ethyoxyl-14-benzoylaconitine and 8-acetyl-14-ethyoxylaconitine were identified firstly as reaction products of aconitine in dilute ethanol, and can thus be used as indicators in quality control of medicinal Aconitum preparations used in Traditional Chinese Medicine.

  16. Analysis of in vitro activity of high dilutions of Euphorbia tirucalli L. in human melanoma cells

    Directory of Open Access Journals (Sweden)

    Teresa Cristina Andrade Leitao Aguiar


    Full Text Available Aveloz (firestick cactus; Euphorbia tirucalli L. belongs to Euphorbiaceae family, characterized by the production of a toxic latex that has corrosive effects on the skin and mucous membranes. Continual topic use of the latex is recommended by popular medicine to treat warts, and epitheliomas. To validate this indication, ultra diluted latex and homeopathic medicine Euphorbia tirucalli were tested in vitro on the proliferation of melanoma cells. Ultra diluted latex was prepared in homeopathic dilutions 5cH, 15cH and 30cH by dilution and agitation (trituration for solid and sucussion for liquid phases using 70º GL (Gay Lussac ethylic alcohol (70º GL EtOH 70ºGL as inert medium according to the guidelines in Farmacopéia Homeopática Brasileira (FHB. Homeopathic medicine Euphorbia tirucalli was prepared from mother-tincture according to the centesimal Hahnemannian method. Solutions 0.5% and 5% of 70ºGL EtOH were succussed and used as control. Human melanoma cells were cultured, treated and monitored by method MTT for 24 to 72 hours. It was observed that 0.5% 70ºGL EtOH solution had little or no effect on the proliferation of melanoma cells (5.1% maximal inhibition in dilution 30cH. Positive correlation was observed in most groups between inhibition of proliferation and diluted preparations, maximal increase (9% was seen in with 5% latex. Moreover, mother-tincture proved to be more active than latex; treatment with 0.5% solution of latex 30cH exhibited 19.7% inhibition, whereas treatment with 0.5% solution of Euphorbia tirucalli 30cH exhibited 32.1% inhibition of cell proliferation (p<0.05. These results suggest that high dilutions of firestick cactus (especially dilution 30cH might have a therapeutic indication in melanoma, further studies are needed in this regard.

  17. Effect of dilution, temperature, and preservatives on the long-term stability of standardized inhalant allergen extracts

    NARCIS (Netherlands)

    Niemeijer, NR; Kauffman, HF; vanHove, W; Dubois, AEJ; deMonchy, JGR

    Background: Although documented stability of allergens used for diagnosis is important, research in this area has been limited. Most studies on extract stability have been of limited duration and discrepancies have been reported between stability test results of in vivo and in vitro methods.

  18. Pre-column dilution large volume injection ultra-high performance liquid chromatography-tandem mass spectrometry for the analysis of multi-class pesticides in cabbages. (United States)

    Zhong, Qisheng; Shen, Lingling; Liu, Jiaqi; Yu, Dianbao; Li, Siming; Yao, Jinting; Zhan, Song; Huang, Taohong; Hashi, Yuki; Kawano, Shin-ichi; Liu, Zhaofeng; Zhou, Ting


    Pre-column dilution large volume injection (PD-LVI), a novel sample injection technique for reverse phase ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), was developed in this study. The PD-LVI UHPLC-MS/MS system was designed by slightly modifying the commercial UHPLC-MS/MS equipment with a mixer chamber. During the procedure of PD-LVI, sample solution of 200μL was directly carried by the organic mobile phase to the mixer and diluted with the aqueous mobile phase. After the mixture was introduced to the UHPLC column in a mobile phase of acetonitrile-water (15/85, v/v), the target analytes were stacked on the head of the column until following separation. Using QuEChERS extraction, no additional steps such as solvent evaporation or residue redissolution were needed before injection. The features of PD-LVI UHPLC-MS/MS system were systematically investigated, including the injection volume, the mixer volume, the precondition time and the gradient elution. The efficiency of this approach was demonstrated by direct analysis of 24 pesticides in cabbages. Under the optimized conditions, low limits of detection (0.00074-0.8 ng/kg) were obtained. The recoveries were in the range of 63.3-109% with relative standard deviations less than 8.1%. Compared with common UHPLC-MS/MS technique, PD-LVI UHPLC-MS/MS showed significant advantages such as excellent sensitivity and reliability. The mechanism of PD-LVI was demonstrated to be based on the column-head stacking effect with pre-column dilution. Based on the results, PD-LVI as a simple and effective sample injection technique of reverse phase UHPLC-MS/MS for the analysis of trace analytes in complex samples showed a great promising prospect.

  19. Stable isotope dilution analysis of orotic acid and uracil in amniotic fluid

    NARCIS (Netherlands)

    Jakobs, C.; Sweetman, L.; Nyhan, W.L.; Gruenke, L.; Craig, J.C.; Wadman, S.K.


    Rapid, sensitive and accurate stable isotope dilution assays were developed for the measurement of orotic acid and uracil in amniotic fluid. The method utilizes [15N2]orotic acid and [15N2]uracil as internal standards, isolation by liquid partition chromatography and quantitation by chemical ionizat

  20. Determination of Glyphosate, its Degradation Product Aminomethylphosphonic Acid, and Glufosinate, in Water by Isotope Dilution and Online Solid-Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (United States)

    Meyer, Michael T.; Loftin, Keith A.; Lee, Edward A.; Hinshaw, Gary H.; Dietze, Julie E.; Scribner, Elisabeth A.


    The U.S. Geological Survey method (0-2141-09) presented is approved for the determination of glyphosate, its degradation product aminomethylphosphonic acid (AMPA), and glufosinate in water. It was was validated to demonstrate the method detection levels (MDL), compare isotope dilution to standard addition, and evaluate method and compound stability. The original method USGS analytical method 0-2136-01 was developed using liquid chromatography/mass spectrometry and quantitation by standard addition. Lower method detection levels and increased specificity were achieved in the modified method, 0-2141-09, by using liquid chromatography/tandem mass spectrometry (LC/MS/MS). The use of isotope dilution for glyphosate and AMPA and pseudo isotope dilution of glufosinate in place of standard addition was evaluated. Stable-isotope labeled AMPA and glyphosate were used as the isotope dilution standards. In addition, the stability of glyphosate and AMPA was studied in raw filtered and derivatized water samples. The stable-isotope labeled glyphosate and AMPA standards were added to each water sample and the samples then derivatized with 9-fluorenylmethylchloroformate. After derivatization, samples were concentrated using automated online solid-phase extraction (SPE) followed by elution in-line with the LC mobile phase; the compounds separated and then were analyzed by LC/MS/MS using electrospray ionization in negative-ion mode with multiple-reaction monitoring. The deprotonated derivatized parent molecule and two daughter-ion transition pairs were identified and optimized for glyphosate, AMPA, glufosinate, and the glyphosate and AMPA stable-isotope labeled internal standards. Quantitative comparison between standard addition and isotope dilution was conducted using 473 samples analyzed between April 2004 and June 2006. The mean percent difference and relative standard deviation between the two quantitation methods was 7.6 plus or minus 6.30 (n = 179), AMPA 9.6 plus or minus 8

  1. Ultra-highly diluted plant extracts of Hydrastis canadensis and Marsdenia condurango induce epigenetic modifications and alter gene expression profiles in HeLa cells in vitro

    Institute of Scientific and Technical Information of China (English)

    Santu Kumar Saha; Sourav Roy; Anisur Rahman Khuda-Bukhsh


    OBJECTIVE: Methylation-specific epigenetic process and gene expression profiles of HeLa cel s treated with ultra-high dilutions (HDs) of two plant extracts, Hydrastis canadensis (HC-30) and Marsdenia condurango (Condu-30), diluted 1060 times, were analyzed against placebo 30C (Pl-30) for alterations in gene profiles linked to epigenetic modifications. METHODS: Separate groups of cel s were subjected to treatment of Condu-30, HC-30, and Pl-30 prepared by serial dilutions and succussions. Global microarray data recorded on Affymetrix platform, using 25-mer probes were provided by iLifeDiscoveries, India. Slides were scanned with 3000 7G microarray scanner and raw data sets were extracted from Cel (raw intensity) files. Analyses of global microarray data profile, differential gene expression, fold change and clusters were made using GeneSpring GX12.5 software and standard normalization procedure. Before microarray study, concentration of RNA (ng/μL), RIN value and rRNA ratio for al the samples were analysed by Agilant Bioanalyzer 2100. Reverse transcriptase polymerase chain reaction (RT-PCR) and quantitative RT-PCR were done for analyzing SMAD-4 expression. Fluorescence-activated cel sorting study was further made to elucidate fate of cel s at divisional stages. Methylation-specific restriction enzyme assay was conducted for ascertaining methylation status of DNA at specific sites. RESULTS: HDs of HC-30 and Condu-30 differential y altered methylation in specific regions of DNA and expression profiles of certain genes linked to carcinogenesis, as compared to Pl-30. Two separate cut sites were found in genomic DNA of untreated and placebo-treated HeLa cel s when digested with McrBC, compared to a single cut observed in Condu-30-treated genomic DNA. SMAD-4 gene expression validated the expression pattern observed in microarray profile. Methylation-specific restriction enzyme assay elucidated differential epigenetic modifications in drug-treated and control cel s

  2. Distribution of the hallucinogens N,N-dimethyltryptamine and 5-methoxy-N,N-dimethyltryptamine in rat brain following intraperitoneal injection: application of a new solid-phase extraction LC-APcI-MS-MS-isotope dilution method. (United States)

    Barker, S A; Littlefield-Chabaud, M A; David, C


    A method for the solid-phase extraction (SPE) and liquid chromatographic-atmospheric pressure chemical ionization-mass spectrometric-mass spectrometric-isotope dilution (LC-APcI-MS-MS-ID) analysis of the indole hallucinogens N,N-dimethyltryptamine (DMT) and 5-methoxy DMT (or O-methyl bufotenin, OMB) from rat brain tissue is reported. Rats were administered DMT or OMB by the intraperitoneal route at a dose of 5 mg/kg and sacrificed 15 min post treatment. Brains were dissected into discrete areas and analyzed by the methods described as a demonstration of the procedure's applicability. The synthesis and use of two new deuterated internal standards for these purposes are also reported.

  3. Comparative analysis of deuterium ions implanted and deuterium atoms saturated at high pressure in pure pd and Pd diluted alloys (United States)

    Didyk, A. Yu.; Kulikauskas, V. S.; Wiśniewski, R.; Wilczynska, T.; Kitowski, K.


    Pd and its diluted alloys (Pd-Ag, Pd-Pt, Pd-Ru, Pd-Rh) were implanted by 25 keV deuterium ions at a fluence interval of (1.2-2.3) × 1022 m-2. The same property alloys were saturated by deuterium atoms using high pressure chamber during long period with temperature stabilization and electrical resistance measurement of standard Pd wire. The post-treatment depth distributions of deuterium and accompanied hydrogen atoms were measured immediately after implantation (ten days) and after definite time period (three months) after saturation with the usage of elastic recoil detection analysis (ERDA). After two months, the measurements were repeated. The comparison of obtained results in both series of studies allowed one to make an important observation of a relative stability of deuterium and hydrogen atoms in pure Pd and its diluted alloys.

  4. From the dilute solution to the pure compound:Extraction strategy based on a multi-stage process of phase separation

    Institute of Scientific and Technical Information of China (English)

    GOUTAUDIER; Christelle; TENU; Richard; COUNIOUX; Jean-Jacques


    It is very rare that a one-step process of extraction leads to the pure compound with a high degree of purity specified by an industrial application.The various stages of a synthesis process and possible secondary reactions may lead to the synthesis of more or less complex and highly diluted solutions.In this work,the rationale and strategy for extraction and purification of a high added value compound are discussed.All the thinking is based on the knowledge and the exploitation of phase diagrams and then developed for different unit operations of the process.The most significant research tools are the experimental data and the modelling of phase equilibrium to estimate the yield of each step of extraction.The significant example chosen involves all the basic methods of phase separation,starting with liquid-vapour equilibrium:stripping of high volatility components and then more or less complex distillation are classically employed.The theoretical plateau number can be deduced from the equilibrium equation curves.The second step is based on the study of the liquid-liquid equilibrium and is an intermediate step for enrichment of the solution when distillation is not possible.A final step based on solid-liquid equilibrium consists of the selective crystallization of the pure product at low temperature,in order to satisfy the requirements of purity and safety imposed by industrial use.The conclusion includes all isolation operations in the form of a general extraction and purification scheme.

  5. Dune formation in dilute phase pneumatic transport system: PIV & PTV based analysis (United States)

    Jhalani, Sumit; Patankar, Atharva; Makawana, Ajay; Bose, Manaswita


    Flow of gas-solid mixture through horizontal conveying section show a large variety of phenomena and is broadly classified into dilute and dense unstable regimes. Different types of instabilities are observed in the dense phase flow and are widely studied in literature; however, clustering instabilities are observed in the very dilute regime of flow with volume fraction 0.001. A recent study has shown that regular, stable dune shaped clusters are formed in a small regime of the dilute phase of conveying. The dunes become unstable as the superficial gas velocity is decreased before it finally leads to the dense mode of conveying. The motivation of the current work is to investigate the velocity distribution on the surface of the stable and unstable dunes and thereby understand the cause behind the formation of the dunes in the conveying section. To that end, particle image and tracking velocimetry techniques are employed with the specific objective to determine the volume fraction and the velocity profile of the solid phase on the stable dune surface. A drastic change in the solid fraction within a few particle diameters from the dune surface suggests that PTV is more appropriate in the bulk whereas PIV is suitable for near surface investigation.

  6. Structural, morphological and magnetic analysis of Cd–Co–S dilute magnetic semiconductor nanofilms

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Suresh [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India); Negi, N.S. [Department of Physics, Himachal Pradesh University, Summer Hill, Shimla, Himachal Pradesh 171005 (India); Katyal, S.C. [Department of Physics, Jaypee Institute of Information Technology, Sec-128, Noida, Uttar Pradesh 201301 (India); Sharma, Pankaj, E-mail: [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India); Sharma, Vineet [Department of Physics and Materials Science, Jaypee University of Information Technology, Waknaghat, Solan, Himachal Pradesh 173234 (India)


    Cd{sub 1−x}Co{sub x}S dilute magnetic semiconductor nanofilms (0≤x≤0.08 at%) deposited by chemical bath deposition have been investigated using grazing angle x-ray diffraction, atomic force microscopy and vibrating sample magnetometer. The introduction of Co{sup 2+} ions in CdS structure induces structural disorders and hence, results in degradation of crystallinity. The crystallite size, interplanar spacing and lattice parameter ratio decrease with increasing Co{sup 2+} concentration in CdS. The diamagnetic state of CdS disappears with increase in Co concentration and films with x>0.02 exhibit ferromagnetism. This may be explained in terms of the spin–orbit interactions and Co{sup 2+} ion induced the lattice defects and phase separation. - Highlights: • Cd{sub 1−x}Co{sub x}S dilute magnetic semiconductor nanofilms (0≤x≤0.08 at%) deposited by CBD. • The diamagnetic state of CdS vanishes for x=0.02. • For x>0.02, dilute magnetic semiconductor nanofilms shows a ferromagnetic state.

  7. Regional water-quality analysis of 2,4-D and dicamba in river water using gas chromatography-isotope dilution mass spectrometry (United States)

    Thurman, E.M.; Zimmerman, L.R.; Aga, D.S.; Gilliom, R.J.


    Gas chromatography with isotope dilution mass spectrometry (GC-MS) and enzyme-linked immunosorbent assay (ELISA) were used in regional National Water Quality Assessment studies of the herbicides, 2,4-D and dicamba, in river water across the United States. The GC-MS method involved solid-phase extraction, derivatized with deutemted 2,4-D, and analysis by selected ion monitoring. The ELISA method was applied after preconcentration with solid-phase extraction. The ELISA method was unreliable because of interference from humic substances that were also isolated by solid-phase extraction. Therefore, GC-MS was used to analyzed 80 samples from river water from 14 basins. The frequency of detection of dicamba (28%) was higher than that for 2,4-D (16%). Concentrations were higher for dicamba than for 2,4-D, ranging from less than the detection limit (<0.05 ??g/L) to 3.77 ??g/L, in spite of 5 times more annual use of 2,4-D as compared to dicamba. These results suggest that 2,4-D degrades more rapidly in the environment than dicamba.

  8. Speciation and reactivity of lead and zinc in heavily and poorly contaminated soils: Stable isotope dilution, chemical extraction and model views. (United States)

    Ren, Zong-Ling; Sivry, Yann; Tharaud, Mickaël; Cordier, Laure; Li, Yongtao; Dai, Jun; Benedetti, Marc F


    Correct characterization of metal speciation and reactivity is a prerequisite for the risk assessment and remedial activity management of contaminated soil. To better understand the intrinsic reactivity of Pb and Zn, nine heavily and poorly contaminated soils were investigated using the combined approaches of chemical extractions, multi-element stable isotopic dilution (ID) method, and multi-surface modelling. The ID results show that 0.1-38% of total Pb and 3-45% of total Zn in the studied soils are isotopically exchangeable after a 3-day equilibration. The intercomparison between experimental and modelling results evidences that single extraction with 0.43 M HNO3 solubilizes part of non-isotopically exchangeable fraction of Pb and Zn in the studied soils, and cannot be used as a surrogate for ID to assess labile Pb and Zn pools in soil. Both selective sequential extraction (SSE) and modelling reveal that Mn oxides are the predominant sorption surface for Pb in the studied soils; while Zn is predicted to be mainly associated with soil organic matter in the soil with low pH and Fe/Mn oxides in the soils with high pH. Multi-surface modelling can provide a reasonable prediction of Pb and Zn adsorption onto different soil constituents for the most of the studied soils. The modelling could be a promising tool to decipher the underlying mechanism that controls metal reactivity in soil, but the submodel for Mn oxides should be incorporated and the model parameters, especially for the 2-pK diffuse layer model for Mn oxides, should be updated in the further studies. Copyright © 2017. Published by Elsevier Ltd.

  9. Cadmium determination in natural waters at the limit imposed by European legislation by isotope dilution and TiO{sub 2} solid-phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Ruiz, Silvia; Quetel, Christophe R. [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); Petrov, Ivan [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); Universite Libre de Bruxelles, Department of Earth and Environmental Sciences, Brussels (Belgium); Vassileva, Emilia [Institute for Reference Materials and Measurements, Joint Research Centre - European Commission, Geel (Belgium); IAEA-Marine Environment Laboratories, Monaco (Monaco)


    The cadmium content in surface water is regulated by the last European Water Framework Directive to a maximum between 0.08 and 0.25 {mu}g L{sup -1} depending on the water type and hardness. Direct measurement of cadmium at this low level is not straightforward in real samples, and we hereby propose a validated method capable of addressing cadmium content below {mu}g L{sup -1} level in natural water. It is based on solid-phase extraction using TiO{sub 2} nanoparticles as solid sorbent (0.05 g packed in mini-columns) to allow the separation and preconcentration of cadmium from the sample, combined to direct isotope dilution and detection by inductively coupled plasma mass spectrometry (ID-ICP-MS). The extraction setup is miniaturised and semi-automated to reduce risks of sample contamination and improve reproducibility. Procedural blanks for the whole measurement process were 5.3 {+-} 2.8 ng kg{sup -1} (1 s) for 50 g of ultrapure water preconcentrated ten times. Experimental conditions influencing the separation (including loading pH, sample flow rates, and acid concentration in the eluent) were evaluated. With isotope dilution the Cd recovery rate does not have to be evaluated carefully. Moreover, the mathematical model associated to IDMS is known, and provides transparency for the uncertainty propagation. Our validation protocol was in agreement with guidelines of the ISO/IEC 17025 standard (chapter 5.4.5). Firstly, we assessed the experimental factors influencing the final result. Secondly, we compared the isotope ratios measured after our separation procedure to the reference values obtained with a different protocol for the digested test material IMEP-111 (mineral feed). Thirdly, we analysed the certified reference material BCR-609 (groundwater). Finally, combined uncertainties associated to our results were estimated according to ISO-GUM guidelines (typically, 3-4% k = 2 for a cadmium content of around 100 ng kg{sup -1}). We applied the developed method to the

  10. Quantification of VX vapor in ambient air by liquid chromatography isotope dilution tandem mass spectrometric analysis of glass bead filled sampling tubes. (United States)

    Evans, Ronald A; Smith, Wendy L; Nguyen, Nam-Phuong; Crouse, Kathy L; Crouse, Charles L; Norman, Steven D; Jakubowski, E Michael


    An analysis method has been developed for determining low parts-per-quadrillion by volume (ppqv) concentrations of nerve agent VX vapor actively sampled from ambient air. The method utilizes glass bead filled depot area air monitoring system (DAAMS) sampling tubes with isopropyl alcohol extraction and isotope dilution using liquid chromatography coupled with a triple-quadrupole mass spectrometer (LC/MS/MS) with positive ion electrospray ionization for quantitation. The dynamic range was from one-tenth of the worker population limit (WPL) to the short-term exposure limit (STEL) for a 24 L air sample taken over a 1 h period. The precision and accuracy of the method were evaluated using liquid-spiked tubes, and the collection characteristics of the DAAMS tubes were assessed by collecting trace level vapor generated in a 1000 L continuous flow chamber. The method described here has significant improvements over currently employed thermal desorption techniques that utilize a silver fluoride pad during sampling to convert VX to a higher volatility G-analogue for gas chromatographic analysis. The benefits of this method are the ability to directly analyze VX with improved selectivity and sensitivity, the injection of a fraction of the extract, quantitation using an isotopically labeled internal standard, and a short instrument cycle time.

  11. Structural characterization and physicochemical properties of protein extracted from soybean meal assisted by steam flash-explosion with dilute acid soaking. (United States)

    Zhang, Yanpeng; Yang, Ruijin; Zhang, Weinong; Hu, Zhixiong; Zhao, Wei


    The aim of this work was to analyze the influence of steam flash-explosion (SFE) with dilute acid soaking pretreatment on the structural characteristics and physiochemical properties of protein from soybean meal (SBM). The pretreatment led to depolymerisation of soy protein isolate (SPI) and formation of new protein aggregation through non-disulfide covalent bonds, which resulted in broader MW distribution of SPI. The analysis of CD spectroscopy showed that the SFE treatment induced minor changes in secondary structure, however, the intrinsic tryptophan fluorescence revealed that acid soaking and SFE treatment pronouncedly altered the tertiary structure of SPI. The protein zeta potential was shown to be increased after SFE treatment attributed to the changes in protein structure and the covalent coupling between carbohydrate and protein. These results contribute to clarifying the mechanisms of the effect of pretreatment on SPI structure, thus moving further toward implementing SFE in the processing chain of SPI.

  12. Phytochemical analysis and antioxidant activities of Trigona Apicalis propolis extract (United States)

    Rosli, Nur Liyana; Roslan, Husniyati; Omar, Eshaifol Azam; Mokhtar, Norehan; Hapit, Nor Hussaini Abdul; Asem, Nornaimah


    Propolis is a resinous substance found in beehives. It provides beneficial effects on human health and has been used to treat many diseases since ancient times. The objectives of this study were to analyze the phytochemical profile of propolis derived from local T. apicalis species and its antioxidant activities. The ethanolic extract of propolis was subjected to HPLC analysis to analyze its phytochemical profile. The propolis extract was later tested for antioxidant capacities by using DPPH radical scavenging assay. TPC and TFC were performed to determine the correlation with its antioxidant activities. TEAC for each serial dilution sample was 2621.15 (4.76 mg/mL), 2050.85 (2.38 mg/mL), 1883.27 (1.19 mg/mL), 1562.67 (0.59 mg/mL), 1327.82 (0.29 mg/mL), 1164.49 (0.15 mg/mL), 983.27 (0.07 mg/mL), and 944.79 (0.04 mg/mL). The results demonstrated that the antioxidant activities of propolis extract were dose dependent. The IC50 of propolis for DPPH assay was 4.27 mg/ml. Correlation values of TPC and TFC against DPPH indicate that the antioxidant activities of propolis extract used in this study could be mainly influenced by the phenolic and flavonoid contents. These findings highlighted the importance of quality analysis in order to ensure the consistency of biological effects or therapy of a natural product, such as propolis.

  13. Phenylboronic Acid Solid Phase Extraction Cleanup and Isotope Dilution Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Florfenicol Amine in Fish Muscles. (United States)

    Sin, Della Wai-Mei; Ho, Clare; Wong, Yiu-Tung


    Florfenicol (FFC) residues in foods are regulated as the sum of florfenicol and its metabolites measured as florfenicol amine (FFA). An isotope dilution LC-MS/MS method utilizing phenylboronic acid (PBA) SPE cleanup is established for the accurate determination of FFA in fish muscles (i.e., salmon and tilapia) after acid catalyzed hydrolysis. Comparisons of the PBA SPE cleanup procedure with other cleanup procedures such as mixed-mode cationic (MCX) SPE and solid supported liquid-liquid extraction were performed. Quantification of FFA in fish muscles was accomplished by using matrix-matched calibration with FFA-D3 as the internal standard. The method was validated with FFA fortified fish muscles at three different levels (50, 100, and 200 μg/kg). Conversion of FFC to FFA by acid catalyzed hydrolysis was evaluated and found to be ≥88%. The recoveries of FFA in fish muscles at the three fortification levels ranged from 89 to 106%, and RSDs were ≤9% in all cases. The LOD values in salmon and tilapia muscles were 0.13 and 1.64 μg/kg, respectively. The LOQ values in salmon and tilapia muscles were 0.29 and 4.13 μg/kg, respectively. This method is suitable for the application in routine control of FFC in fishes according to its residue definition.

  14. Antimicrobial activity and phytochemical analysis of crude extracts and essential oils from medicinal plants. (United States)

    Silva, N C C; Barbosa, L; Seito, L N; Fernandes, A


    We aimed to establish a phytochemical analysis of the crude extracts and performed GC-MS of the essential oils (EOs) of Eugenia uniflora L. (Myrtaceae) and Asteraceae species Baccharis dracunculifolia DC, Matricaria chamomilla L. and Vernonia polyanthes Less, as well as determining their antimicrobial activity. Establishment of the minimal inhibitory concentrations of the crude extracts and EOs against 16 Staphylococcus aureus and 16 Escherichia coli strains from human specimens was carried out using the dilution method in Mueller-Hinton agar. Some phenolic compounds with antimicrobial properties were established, and all EOs had a higher antimicrobial activity than the extracts. Matricaria chamomilla extract and E. uniflora EO were efficient against S. aureus strains, while E. uniflora and V. polyanthes extracts and V. polyanthes EO showed the best antimicrobial activity against E. coli strains. Staphylococcus aureus strains were more susceptible to the tested plant products than E. coli, but all natural products promoted antimicrobial growth inhibition.

  15. Structural, morphological and magnetic analysis of Cd-Co-S dilute magnetic semiconductor nanofilms (United States)

    Kumar, Suresh; Negi, N. S.; Katyal, S. C.; Sharma, Pankaj; Sharma, Vineet


    Cd1-xCoxS dilute magnetic semiconductor nanofilms (0≤x≤0.08 at%) deposited by chemical bath deposition have been investigated using grazing angle x-ray diffraction, atomic force microscopy and vibrating sample magnetometer. The introduction of Co2+ ions in CdS structure induces structural disorders and hence, results in degradation of crystallinity. The crystallite size, interplanar spacing and lattice parameter ratio decrease with increasing Co2+ concentration in CdS. The diamagnetic state of CdS disappears with increase in Co concentration and films with x>0.02 exhibit ferromagnetism. This may be explained in terms of the spin-orbit interactions and Co2+ ion induced the lattice defects and phase separation.

  16. Theoretical analysis and numerical computation of dilute solid/liquid two_phase pipe flow

    Institute of Scientific and Technical Information of China (English)


    Starting with the kinetic theory for dilute solid/liquid two_phase flow, a mathematical model is established to predict the flow in a horizontal square pipe and the predictions are compared with LDV measurements. The present model predicts correctly two types of patterns of the vertical distribution of particle concentration observed in experiments, and also gives different patterns of the distribution of particle fluctuating energy. In the core region of the pipe, the predicted mean velocity of particles is smaller than that of liquid, but near the pipe bottom the reverse case occurs. In addition, full attention is paid to the mechanism for the vertical distribution of the average properties of particles such as concentration and mean velocity. From the kinetic_theory point of view, the cause of formation for different patterns of the vertical concentration distribution is not only related to the lift force exerted on a particle, but also related to the distribution of particle fluctuating energy.

  17. Isotope dilution analysis of Ca and Zr in apatite and zircon (U-Th)/He chronometry (United States)

    Guenthner, William R.; Reiners, Peter W.; Chowdhury, Uttam


    Because radiation damage influences He diffusivity, correlations between (U-Th)/He ages and effective uranium (eU, eU = U + 0.235 × Th) concentrations of single apatite and zircon grains are important for understanding thermal histories. Here we describe a method for quantifying eU concentrations in apatite and zircon grains using isotope dilution ICP-MS measurements of Zr and Ca and stoichiometry of zircon (ZrSiO4) and apatite (Ca5(PO4)3F) to obtain grain masses. Combined with independent U and Th measurements, these yield eU concentrations not based on the traditional morphologic measurements and assumptions. Additional benefits of this method include correct identification of an apatite or zircon and volume estimates for crystal shards. In some cases, this method gives eU concentrations consistent with those calculated with the morphologic approach, but often significant differences are observed between concentrations calculated from the two methods. Differences in eU concentrations for our apatite grains are greater and less than morphology estimates, and the majority are between 0.7 and 31%. With the exception of two grains, all of our zircon grains have differences between 3 and 34% less than morphology estimates. These differences could result from incorrect grain width measurements, mischaracterized grain shape, or incorrect volume calculations of the pure mineral phase due to inclusions. These morphologic errors—combined with evidence for the accuracy of our isotope dilution method from analyses of reference materials—suggest that eU concentrations calculated from morphology may often be significantly inaccurate. Finally, we demonstrate that differences between the two measurements of eU cause age-eU correlation variations for representative thermal histories.

  18. Quantitative analysis of metabolites in complex biological samples using ion-pair reversed-phase liquid chromatography-isotope dilution tandem mass spectrometry. (United States)

    Seifar, Reza M; Zhao, Zheng; van Dam, Jan; van Winden, Wouter; van Gulik, Walter; Heijnen, Joseph J


    A rapid, sensitive and selective ion-pair reversed-phase liquid chromatography-electrospray ionization isotope dilution tandem mass spectrometry (IP-LC-ESI-ID-MS/MS) was developed for quantitative analysis of free intracellular metabolites in cell cultures. As an application a group of compounds involved in penicillin biosynthesis pathway of Penicillium chrysogenum cells, such as penicillin G (PenG), 6-aminopenicillanic acid (6-APA), benzylpenicilloic acid (PIO), ortho-hydroxyphenyl acetic acid (o-OH-PAA), phenylacetic acid (PAA), 6-oxopipeidine-2-carboxylic acid (OPC), 8-hydroxypenicillic acid (8-HPA), L-alpha-(delta-aminoadipyl)-L-alpha-cystenyl-D-alpha-valine (ACV) and isopenicillin N (IPN) were chosen. (13)C-labeled analogs of the metabolites were added to the sample solutions as internal standards (I.S.). Sample mixtures were analyzed without any sample pretreatment. No extraction recovery check was needed because I.S. was added to the cell samples before extraction process. The method showed excellent precision (relative standard deviation (RSD)

  19. Isotope dilution analysis for urinary fentanyl and its main metabolite, norfentanyl, in patients by isotopic fractionation using capillary gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Sera, Shoji; Goromaru, Tsuyoshi [Fukuyama Univ., Hiroshima (Japan). Faculty of Pharmacy and Pharmaceutical Sciences; Sameshima, Teruko; Kawasaki, Koichi; Oda, Toshiyuki


    Isotope dilution analysis was applied to determine urinary excretion of fentanyl (FT) and its main metabolite, norfentanyl (Nor-FT), by isotopic fractionation using a capillary gas chromatograph equipped with a surface ionization detector (SID). Urinary FT was determined quantitatively in the range of 0.4-40 ng/ml using deuterium labeled FT (FT-{sup 2}H{sub 19}), as an internal standard. We also performed isotope dilution analysis of Nor-FT in urine. N-Alkylation was necessary to sensitively detect Nor-FT with SID. Methyl derivative was selected from 3 kinds of N-alkyl derivatives to increase sensitivity and peak resolution, and to prevent interference with urinary compound. Nor-FT concentration was quantitatively determined in the range of 10-400 ng/ml using deuterium labeled Nor-FT (Nor-FT-{sup 2}H{sub 10}). No endogenous compounds or concomitant drugs interfered with the detection of FT and Nor-FT in the urine of patients. The present method will be useful for pharmacokinetic studies and the evaluation of drug interactions in FT metabolism. (author)

  20. Comparative techno-economic analysis of steam explosion, dilute sulfuric acid, ammonia fiber explosion and biological pretreatments of corn stover. (United States)

    Baral, Nawa Raj; Shah, Ajay


    Pretreatment is required to destroy recalcitrant structure of lignocelluloses and then transform into fermentable sugars. This study assessed techno-economics of steam explosion, dilute sulfuric acid, ammonia fiber explosion and biological pretreatments, and identified bottlenecks and operational targets for process improvement. Techno-economic models of these pretreatment processes for a cellulosic biorefinery of 113.5 million liters butanol per year excluding fermentation and wastewater treatment sections were developed using a modelling software-SuperPro Designer. Experimental data of the selected pretreatment processes based on corn stover were gathered from recent publications, and used for this analysis. Estimated sugar production costs ($/kg) via steam explosion, dilute sulfuric acid, ammonia fiber explosion and biological methods were 0.43, 0.42, 0.65 and 1.41, respectively. The results suggest steam explosion and sulfuric acid pretreatment methods might be good alternatives at present state of technology and other pretreatment methods require research and development efforts to be competitive with these pretreatment methods. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Analysis Method of 241Pu Radioactivity by Isotope Dilution-Extraction Liquid Scintillation Spectrometer

    Institute of Scientific and Technical Information of China (English)


    <正>241Pu is the only pure β emitter with the maximum energy of 20.81 keV in plutonium isotopes of 238Pu, 239Pu, 240Pu and 242Pu, in which 241Pu is mostly specific radioactivity because its half-life is 14.29 a.

  2. Flow cytometric analysis of the inhibition of human basophil activation by histamine high dilutions – a replication study

    Directory of Open Access Journals (Sweden)

    Chantal Wälchli


    perform in order to reduce the possibility of artifacts but was omitted in the former study. Conclusions: Laboratory independent replication of homeopathic basic research experiments is still a challenge. Assuming that the results formerly obtained with this model were not due to systematic errors, the quest identifying the crucial factors for successful reproducibility is open for future research. Keywords: Human basophils; histamine; high dilutions; flow cytometry Reference: [1] Sainte-Laudy J, Belon P. Improvement of flow cytometric analysis of basophil activation inhibition by high histamine dilutions. A novel basophil specific marker: CD 203c. Homeopathy. 2006;95:3-8.

  3. Determination of eugenol in fish and shrimp muscle tissue by stable isotope dilution assay and solid-phase extraction coupled gas chromatography-triple quadrupole mass spectrometry. (United States)

    Li, Jincheng; Liu, Huan; Wang, Chaoying; Wu, Lidong; Liu, Dan


    In this study, we developed a new method for the accurate quantification of eugenol in fish samples based on stable isotope dilution assay (SIDA) and solid-phase extraction (SPE) coupled gas chromatography-triple quadrupole mass spectrometry (SIDA-SPE-GC-MS/MS). Due to the difference of matrix effect (ME), it was difficult to determine accurately the level of eugenol residue in different fish and shrimp samples based on external standard calibration method. SIDA was applied to compensate matrix effect (ME) that eugenol-d3 was used as internal standard (IS). Freshwater fish (carp, channel catfish), marine fish (turbot), and shrimp (Penaeus vannawei) were used for the method validation. The average recoveries of eugenol were in the range of 94.7 to 109.78 % when the spiking levels were 10, 50, and 200 μg kg(-1). The inter-day and intra-day precisions were in the range of 1.15-8.19 and 0.71-8.45 %. The limit of detection (LOD) and the limit of quantification (LOQ) were approximately 2.5 and 5.0 μg kg(-1). This method was applied to the real fish samples assay obtained from aquaculture markets in Beijing, China. Eugenol residue was found in two fish samples with the levels at 6.2 and 7.7 μg kg(-1), respectively. Graphical abstract Determination of eugenol in fish and shrimp muscle tissue.

  4. Resonance Extraction from the SAID Analysis

    CERN Document Server

    Workman, Ron


    Resonances are extracted from a number of energy-dependent and single-energy fits to scattering data. The influence of recent, precise EPECUR data is investigated. Results for the single-energy fits are derived using the L+P method of analysis and are compared to those obtained using contour integration applied to the global energy-dependent fits.

  5. LC-HR-MS/MS standard urine screening approach: Pros and cons of automated on-line extraction by turbulent flow chromatography versus dilute-and-shoot and comparison with established urine precipitation. (United States)

    Helfer, Andreas G; Michely, Julian A; Weber, Armin A; Meyer, Markus R; Maurer, Hans H


    Comprehensive urine screening for drugs and metabolites by LC-HR-MS/MS using Orbitrap technology has been described with precipitation as simple workup. In order to fasten, automate, and/or simplify the workup, on-line extraction by turbulent flow chromatography and a dilute-and-shoot approach were developed and compared. After chromatographic separation within 10min, the Q-Exactive mass spectrometer was run in full scan mode with positive/negative switching and subsequent data dependent acquisition mode. The workup approaches were validated concerning selectivity, recovery, matrix effects, process efficiency, and limits of identification and detection for typical drug representatives and metabolites. The total workup time for on-line extraction was 6min, for the dilution approach 3min. For comparison, the established urine precipitation and evaporation lasted 10min. The validation results were acceptable. The limits for on-line extraction were comparable with those described for precipitation, but lower than for dilution. Thanks to the high sensitivity of the LC-HR-MS/MS system, all three workup approaches were sufficient for comprehensive urine screening and allowed fast, reliable, and reproducible detection of cardiovascular drugs, drugs of abuse, and other CNS acting drugs after common doses.

  6. Extraction and elemental analysis of Coleus forskohlii extract


    Haritha Kanne; Narayan Pandurang Burte; Prasanna, V; Ravi Gujjula


    Background: Coleus forskohlii Willd. is a popular traditional medicine used since ancient times for treatment of heart diseases, abdominal colic and respiratory disorders. Objective: The aim of this study was to characterize the root extract of the medicinal plant Coleus forskohlii. Materials and Methods: Dry roots of C. forskohlii were used to extract Forskolin using toluene as a solvent. Thus, obtained extract of C. forskohlii was standardized to 30% and used for further studies. Results: T...

  7. Simultaneous analysis of phthalates, adipate and polycyclic aromatic hydrocarbons in edible oils using isotope dilution-gas chromatography-mass spectrometry. (United States)

    Oh, Min-Seok; Lee, Seon-Hwa; Moon, Myeong Hee; Lee, Dong Soo; Park, Hyun-Mee


    A method for simultaneous determination of 12 priority phthalates, adipate and polycyclic aromatic hydrocarbons (PAHs) in edible oils by isotope dilution-gas chromatography-mass spectrometry (ID-GC-MS) was developed for fast, accurate and trace analysis. The extraction and clean-up procedures were optimised, and using stable isotope-labelled internal standards for each analyte, relative standard deviations (RSDs) of 0.92-10.6% and spiked sample recoveries of 80.6-97.8% were obtained. Limits of detection for PAHs were in the range of 0.15-0.77 µg/kg and those for phthalates were in the range of 4.6-10.0 µg/kg. The calibration curves exhibited good linearities with regression coefficients of R(2) ≥ 0.99. Twelve edible oils were examined to evaluate the efficiency of this method. Among the 12 analytes, dibutyl phthalates (DBP), diethylhexyl phthalates (DEHP), diethylhexyl adipate (DEHA), benzo[a]anthracene (B[a]A), chrysene (Chry) and benzo[b]fluoranthene (B[b]F) were detected in the range of 1.17-806 µg/kg.

  8. Evaluation and validation of a single-dilution potency assay based upon serology of vaccines containing diphtheria toxoid: statistical analysis

    NARCIS (Netherlands)

    Marsman FR; Akkermans AM; Hendriksen CFM; de Jong WH


    This document presents the results of a validation study to the use of a single dilution assay in potency testing of the diphtheria component of DPT-polio vaccines. Based on historical data of multi-dilution assays on 27 consecutive batches a simulation study was performed to test the actual perfor

  9. Analysis of antioxidants extracted from polypropylene by supercritical fluid extraction. (United States)

    Garde, J A; Catalá, R; Gavara, R


    Maximal potential migration of six antioxidants (AO) from five polypropylene (PP) formulations was determined by two supercritical fluid extraction (SFE) procedures, both of which contained static and dynamic steps. All analytical conditions affecting the extraction were studied and optimized using Irgafos 168 as standard. SFE was more efficient as temperature and fluid density increased. During the static step in which the samples were exposed to the fluid without flux, the introduction of hexane and methanol as fluid modifiers significantly improved the extraction. Hexane appears to facilitate polymer swelling while methanol solvates the antioxidants. In the dynamic step (in which the extraction actually occurs) time is the key parameter. Extraction for 90 min results in an efficiency of around 75%. The introduction of modifiers during this step (by an HPLC-SFE procedure) did not produce any significant improvement. When SFE was carried out on all samples, extraction efficiency was around 75% except for Irganox 1010 and Hostanox O3. The large molecular volume of these antioxidants may be responsible for the considerable reduction of extraction efficiency. Particle size and shape of polymer sample were also important. The greater the surface to volume ratio the greater the extraction efficiency.

  10. Analysis of particles produced by oxidation of dilute xylene in air under electron beam irradiation (United States)

    Hakoda, Teruyuki; Goto, Hitoshi; Shimada, Akihiko; Ochi, Masafumi; Kojima, Takuji


    The generator of electron beams with energies of 55 keV (max.) and currents of 0.50 mA (max.) was developed as an irradiation source for the analysis of particles produced from aromatic hydrocarbons under EB irradiation. The oxidation process of o-xylene in air and the characteristic of particles produced from xylene were examined by EB irradiation. The particles of products were analyzed under less their coagulation. The use of this EB generator enables to examine the characteristics of particles under irradiation with their analysis immediately after irradiation.

  11. Extraction and analysis of polyphenols: recent trends. (United States)

    Ajila, C M; Brar, S K; Verma, M; Tyagi, R D; Godbout, S; Valéro, J R


    In recent years, there has been an increasing interest in diets rich in fruits and vegetables and this is mostly due to their presumed role in the prevention of various degenerative diseases, such as cancer and cardiovascular diseases. This is mainly due to the presence of bioactive compounds, such as polyphenols, carotenoids, among others. Polyphenols are one of the main classes of secondary metabolites derived from plants offering several health benefits resulting in their use as functional foods. Prior to the use of these polyphenols in specific applications, such as food, pharmaceutical, and the cosmetic industries, they need to be extracted from the natural matrices, then analyzed and characterized. The development of an efficient procedure for the extraction, proper analysis, and characterization of phenolic compounds from different sources is a challenging task due to the structural diversity of phenolic compounds, a complex matrix, and their interaction with other cellular components. In this light, this review discusses different methods of extraction, analysis, and the structural characterization of polyphenolic compounds.

  12. Clinical Roles of Lung Volumes Detected by Body Plethysmography and Helium Dilution in Asthmatic Patients: A Correlation and Diagnosis Analysis (United States)

    Luo, Jian; Liu, Dan; Chen, Guo; Liang, Binmiao; Liu, Chuntao


    Roles of lung volumes in asthma remain controversial. We aimed to evaluate the efficacy of lung volumes in differentiating asthma severity levels. Consecutive outpatients with chronic persistent asthma were enrolled, and body plethysmography (BP) and helium dilution (HD) were performed simultaneously to extract RV%pred, TLC%pred, and RV/TLC. Significant negative correlations were found between FEV1%pred and RV%pred (r = −0.557, P TLC%pred (r = −0.387, P TLC (r = −0.485, P TLC). In mild and moderate asthma, AUC of RV%pred detected by BP and ΔTLC%pred was 0.723 (95%CI 0.571–0.874, P = 0.005) and 0.739 (95%CI 0.607–0.872, P = 0.002) with sensitivity and specificity being 79.41% and 88.24%, and 65.22% and 56.52% at cut-off of 145.40% and 14.23%, respectively. In moderate and severe asthma, AUC of RV%pred detected by BP and ΔTLC%pred was 0.782 (95%CI 0.671–0.893, P < 0.001) and 0.788 (95%CI 0.681–0.894, P < 0.002) with sensitivity and specificity being 77.78% and 97.22%, and 73.53% and 52.94% at cut-off of 179.85% and 20.22%, respectively. In conclusion, lung volumes are reliable complement of FEV1 in identifying asthma severity levels. PMID:28098214

  13. Analysis of stability of a planar solid-liquid interface in a dilute binary alloy (United States)

    Laxmanan, V.


    This paper reconsiders the question of stability of a planar solid-liquid interface in an undercooled alloy melt without making the restrictive assumption of no heat flow in the solid (i.e., Gs = 0). The results of this analysis indicate that, provided the thermal gradient on the solid side of the interface, Gs, is positive, stability can be achieved in an undercooled alloy melt for growth rates R greater than Ra (where Ra is the absolute stability limit of Mullins and Sekerka, 1964). Thus, the absolute stability criterion for steady-state planar growth in an undercooled alloy melt is the same as derived earlier by Mullins and Sekerka for directional solidification. Relaxing the restrictive assumption of Gs = 0 also reveals that there is a regime of stability for low growth rates and low supercoolings.

  14. Study of the matrix effects and sample dilution influence on the LC-ESI-MS/MS analysis using four derivatization reagents. (United States)

    Oldekop, Maarja-Liisa; Herodes, Koit; Rebane, Riin


    For liquid chromatographic analysis of amino acids involving derivatization and mass-spectrometric detection, it becomes more important to evaluate the presence of matrix effects in complex samples. This is somewhat complicated for amino acid analysis where analyte free sample matrix is often unavailable. In this work, matrix effects were investigated using post-column infusion method for 9-fluorenylmethyl chloroformate (FMOC-Cl) derivatives of β-Ala, Gly and Phe and diethyl ethoxymethylenemalonate (DEEMM) derivative of β-Ala. While for DEEMM derivatives, the main signal suppression was due to the borate buffer, in case of FMOC-Cl, other FMOC-derivatives caused signal suppression. Analysis of amino acids in tea and honey with DEEMM, FMOC-Cl, p-N,N,N-trimethylammonioanilyl N'-hydroxysuccinimidyl carbamate iodide (TAHS) and dansyl chloride (DNS) showed that amino acid concentrations found with different reagents do not agree well. Sample dilution experiments indicated that the sample matrix affected the analysis results obtained with DEEMM the least, but with FMOC-Cl, TAHS and DNS, sample dilution had an influence on the results. When sample dilution and extrapolative dilution approach were applied on the latter results, an agreement of amino acid concentrations measured with different reagents was achieved within relative standard deviation (RSD) of 22% for most cases.

  15. Kinetic and economic analysis of reactive capture of dilute carbon dioxide with Grignard reagents. (United States)

    Dowson, G R M; Dimitriou, I; Owen, R E; Reed, D G; Allen, R W K; Styring, P


    Carbon Dioxide Utilisation (CDU) processes face significant challenges, especially in the energetic cost of carbon capture from flue gas and the uphill energy gradient for CO2 reduction. Both of these stumbling blocks can be addressed by using alkaline earth metal compounds, such as Grignard reagents, as sacrificial capture agents. We have investigated the performance of these reagents in their ability to both capture and activate CO2 directly from dried flue gas (essentially avoiding the costly capture process entirely) at room temperature and ambient pressures with high yield and selectivity. Naturally, to make the process sustainable, these reagents must then be recycled and regenerated. This would potentially be carried out using existing industrial processes and renewable electricity. This offers the possibility of creating a closed loop system whereby alcohols and certain hydrocarbons may be carboxylated with CO2 and renewable electricity to create higher-value products containing captured carbon. A preliminary Techno-Economic Analysis (TEA) of an example looped process has been carried out to identify the electrical and raw material supply demands and hence determine production costs. These have compared broadly favourably with existing market values.

  16. Analysis of Water Extraction From Lunar Regolith (United States)

    Hegde, U.; Balasubramaniam, R.; Gokoglu, S.


    Distribution of water concentration on the Moon is currently an area of active research. Recent studies suggest the presence of ice particles, and perhaps even ice blocks and ice-cemented regolith on the Moon. Thermal extraction of the in-situ water is an attractive means of sa tisfying water requirements for a lunar mission. In this paper, a model is presented to analyze the processes occurring during the heat-up of icy regolith and extraction of the evolved water vapor. The wet regolith is assumed to be present in an initially evacuated and sealed cell which is subsequently heated. The first step of the analysis invol ves calculating the gradual increase of vapor pressure in the closed cell as the temperature is raised. Then, in the second step, the cell is evacuated to low pressure (e.g., vacuum), allowing the water vapor to leave the cell and be captured. The parameters affecting water vap or pressure build-up and evacuation for the purpose of extracting water from lunar regolith are discussed in the paper. Some comparisons wi th available experimental measurements are also made.

  17. Supercritical extraction of oleaginous: parametric sensitivity analysis

    Directory of Open Access Journals (Sweden)

    Santos M.M.


    Full Text Available The economy has become universal and competitive, thus the industries of vegetable oil extraction must advance in the sense of minimising production costs and, at the same time, generating products that obey more rigorous patterns of quality, including solutions that do not damage the environment. The conventional oilseed processing uses hexane as solvent. However, this solvent is toxic and highly flammable. Thus the search of substitutes for hexane in oleaginous extraction process has increased in the last years. The supercritical carbon dioxide is a potential substitute for hexane, but it is necessary more detailed studies to understand the phenomena taking place in such process. Thus, in this work a diffusive model for semi-continuous (batch for the solids and continuous for the solvent isothermal and isobaric extraction process using supercritical carbon dioxide is presented and submitted to a parametric sensitivity analysis by means of a factorial design in two levels. The model parameters were disturbed and their main effects analysed, so that it is possible to propose strategies for high performance operation.

  18. SPS extraction kicker magnet thermal analysis

    CERN Document Server

    Timmins, M


    As the SPS accelerator will be used for the CNGS project and as LHC injector, the proton beams passing through its extraction kickers will have a much higher intensity than in the past. The image currents generated by this beam may provoke a temperature increase in the magnet's ferrite core to temperatures above the Curie temperature, unless the heat produced is effectively removed. A further complication arises from the fact that a high voltage is applied to the ferrites. The solution adopted consists in transferring the heat via Aluminium Nitride insulators to a water cooling circuit. The heat transfer analysis and the calculated thermal distribution of the magnet are presented.

  19. Limiting dilution analysis of alloantigen-reactive cells which respond to allogeneic lymphocytes in human MLC and PLT. (United States)

    Singal, D P; Naipaul, N; Joseph, S


    We have determined the frequency of the alloantigen-reactive cells (ARC) in human MLC and PLT by the limiting dilution analysis. In PLT, the frequency of the ARC to the original sensitizing donor ranged between 1:32 to 1:62, an increase of six to nine-fold after priming in MLC. The MLC primed populations were also enriched (three to five fold) for the ARC responding to the PL-positive allogeneic donors. The incidence of the ARC was 1:62 to 1:118 with donors positive for the sensitizing HLA-DRw antigen and 1:77 to 1:144 with donors negative for the specific HLA-DRw determinant. The results from experiments utilizing pooled stimulating cells from the original and allogeneic donors suggest that same subpopulation of cells responds to the sensitizing HLA-DRw determinant, whether it is presented by the specific stimulator or by a third-party allogeneic donor. On the other hand, different subpopulations of alloreactive cells respond to different alloantigens. In MLC experiments between HLA-identical siblings, the incidence of the ARC ranged between 1:995 to 1:1673. The responses of the ARC to non-HLA antigens were observed under conditions where responder cells were limiting. Also, the responses of the limiting numbers of responding cells were inhibited by mitomycin-treated autologous lymphocytes. Nonresponse in MLC combinations with higher responder cell numbers was not due to small numbers of stimulating cells.

  20. Limiting-dilution analysis for the determination of leukemic cell frequencies after bone marrow decontamination with mafosfamide or merocyanine 540

    Energy Technology Data Exchange (ETDEWEB)

    Porcellini, A.; Talevi, N.; Marchetti-Rossi, M.T.; Palazzi, M.; Manna, A.; Sparaventi, G.; Delfini, C.; Valentini, M.


    To stimulate a leukemia remission marrow, cell suspensions of normal human bone marrow were mixed with human acute lymphoblastic or myelogenous leukemic cells of the CCRF-SF, Nalm-6, and K-562 lines. The cell mixtures were incubated in vitro with mafosfamide (AZ) or with the photoreactive dye merocyanine 540 (MC-540). A quantity of 10(4) cells of the treated suspensions was dispensed into microculture plates, and graded cell numbers of the line used to contaminate the normal marrow were added. Limiting-dilution analysis was used to estimate the frequency of leukemia cells persisting after treatment with the decontaminating agents. Treatment with AZ or MC-540 produced a total elimination (ie, 6 logs or 5.3 logs respectively) of B cell acute leukemia cells (CCRF-SB), whereas nearly 1.7 logs and 2 logs of K-562 acute myelogenous blasts were still present in the cell mixtures after treatment with MC-540 and AZ, respectively. Treatment of the Nalm-6-contaminated cell mixtures with AZ resulted in 100% elimination of clonogenic cells, whereas nearly 80% decontamination was obtained with MC-540. Our results suggest that treatment with AZ could be an effective method of eliminating clonogenic tumor cells from human bone marrow. MC-540, shown by previous studies to spare sufficient pluripotential stem cells to ensure hemopoietic reconstitution in the murine model and in clinical application, has comparable effects and merits trials for possible clinical use in autologous bone marrow transplantation.

  1. Studies on the analysis of 25-hydroxyvitamin D{sub 3} by isotope-dilution liquid chromatography–tandem mass spectrometry using enzyme-assisted derivatisation

    Energy Technology Data Exchange (ETDEWEB)

    Abdel-Khalik, Jonas, E-mail: [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Crick, Peter J. [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Carter, Graham D. [DEQAS, Imperial College Healthcare NHS Trust, Clinical Biochemistry Department, Charing Cross Hospital, Fulham Palace Rd, London W6 8RF (United Kingdom); Makin, Hugh L. [Barts and the Royal London School of Medicine and Dentistry, Queen Mary University of London, London E1 2AD (United Kingdom); Wang, Yuqin [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Griffiths, William J., E-mail: [Institute of Mass Spectrometry, College of Medicine, Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom)


    Highlights: • New method for the analysis of 25-hydroxyvitamin D{sub 3} exploiting Girard P derivatisation. • Method also applicable to vitamin D{sub 3}, 1α,25- and 24,25-dihydroxyvitamin D{sub 3}. • By modification of the method 3-epi-25-hydroxyvitamin D{sub 3} can also be analysed. - Abstract: The total serum concentration of 25-hydroxyvitamins D (25-hydroxyvitamin D{sub 3} and 25-hydroxyvitamin D{sub 2}) is currently used as an indicator of vitamins D status. Vitamins D insufficiency is claimed to be associated with multiple diseases, thus accurate and precise reference methods for the quantification of 25-hydroxyvitamins D are needed. Here we present a novel enzyme-assisted derivatisation method for the analysis of vitamins D metabolites in adult serum utilising 25-[26,26,26,27,27,27-{sup 2}H{sub 6}]hydroxyvitamin D{sub 3} as the internal standard. Extraction of 25-hydroxyvitamins D from serum is performed with acetonitrile, which is shown to be more efficient than ethanol. Cholesterol oxidase is used to oxidize the 3β-hydroxy group in the vitamins D metabolites followed by derivatisation of the newly formed 3-oxo group with Girard P reagent. 17β-Hydroxysteroid dehydrogenase type 10 is shown to oxidize selectively the 3α-hydroxy group in the 3α-hydroxy epimer of 25-hydroxyvitamin D{sub 3}. Quantification is achieved by isotope-dilution liquid chromatography–tandem mass spectrometry. Recovery experiments for 25-hydroxyvitamin D{sub 3} performed on adult human serum give recovery of 102–106%. Furthermore in addition to 25-hydroxyvitamin D{sub 3}, 24,25-dihydroxyvitamin D{sub 3} and other uncharacterised dihydroxy metabolites, were detected in adult human serum.

  2. Analysis of advanced glycation endproducts in dairy products by isotope dilution liquid chromatography-electrospray tandem mass spectrometry. The particular case of carboxymethyllysine. (United States)

    Delatour, Thierry; Hegele, Jörg; Parisod, Véronique; Richoz, Janique; Maurer, Sarah; Steven, Matthew; Buetler, Timo


    A fully validated multiple-transition recording isotope dilution liquid chromatography-electrospray tandem mass spectrometry (LC-MS/MS) method for the simultaneous quantitative determination of N(epsilon)-carboxymethyllysine (CML) and lysine in dairy products is described. Internal standards were [N-1',2'-(13)C(2)]CML and [1,2,3,4,5,6-(13)C(6)-2,6-(15)N(2)]lysine, and the method was validated by evaluating the selectivity, linearity, precision (repeatability and reproducibility) and trueness, using both powder and liquid products. For liquid dairy products, the repeatability and reproducibility was 2.79% and 11.0%, while 4.85% and 4.92% were determined for powder dairy products, respectively. The trueness of the method ranged from -9.6% to -3.6% for powder and from -0.99% to 6.8% for liquid dairy products. The limit of detection for CML was estimated to be 8 ng CML per mg protein while the limit of quantification was 27 ng CML per mg protein. The method encompasses a proteolytic cleavage mediated by enzymatic digestion to reach a complete release of the amino acids prior to a sample cleanup based on solid phase extraction, and followed by LC-MS/MS analysis of CML and lysine residues. To ensure a suitable performance of the enzymatic digestion, CML measurements were compared to values obtained with an acid hydrolysis-mediated proteolysis. Finally, the method was employed for the analysis of CML in various dairy products. The values compare well to the data available in the literature when similar methods were used, even if some discrepancies were observed upon comparison with the results obtained by other techniques such as enzyme-linked immunosorbent assay and GC-MS.

  3. Biosynthesis of 15N-labeled cylindrospermopsin and its application as internal standard in stable isotope dilution analysis. (United States)

    Kittler, Katrin; Hoffmann, Holger; Lindemann, Franziska; Koch, Matthias; Rohn, Sascha; Maul, Ronald


    Cylindrospermopsin (CYN) is a cyanobacterial toxin associated with human and animal poisonings. Due to its toxicity in combination with its widespread occurrence, the development of reliable methods for selective, sensitive detection and accurate quantification is mandatory. Liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis using stable isotope dilution analysis (SIDA) represents an ideal tool for this purpose. U-[(15)N5]-CYN was synthesized by culturing Aphanizomenon flos-aquae in Na(15)NO3-containing cyanobacteria growth medium followed by a cleanup using graphitized carbon black columns and mass spectrometric characterization. Subsequently, a SIDA-LC-MS/MS method for the quantification of CYN in freshwater and Brassica matrices was developed showing satisfactory performance data. The recovery ranged between 98 and 103 %; the limit of quantification was 15 ng/L in freshwater and 50 μg/kg dry weight in Brassica samples. The novel SIDA was applied for CYN determination in real freshwater samples as well as in kale and in vegetable mustard exposed to toxin-containing irrigation water. Two of the freshwater samples taken from German lakes were found to be CYN-contaminated above limit of quantification (17.9 and 60.8 ng/L). CYN is systemically available to the examined vegetable species after exposure of the rootstock leading to CYN mass fractions in kale and vegetable mustard leaves of 15.0 μg/kg fresh weight and 23.9 μg/kg fresh weight, respectively. CYN measurements in both matrices are exemplary for the versatile applicability of the developed method in environmental analysis.


    Directory of Open Access Journals (Sweden)



    Full Text Available Tabernaemontana divaricata is a common shrub found in the tropical regions and is often used for medicinal purposes, particularly the flowers of the plant. The present study is conducted to compare and identify the phytochemical constituents by Thin Layer Chromatography (TLC and Qualitative Phytochemical analysis and to determine the anthelmentic activity of fresh and dried flower extract of Tabernaemontana divaricata. The extract is obtained using two different methods like cold maceration and hot solvent extraction by using soxhlet apparatus, first with petroleum ether followed by hydroalcohol as solvents. The preliminary phytochemical analysis of the extract indicated the presence of Alkaloids, Flavanoids, Steroids, Proteins, Carbohydrates and Tannins. The Rf value of TLC is calculated and compared with standard values and analysis proved the presence of the phytochemical constituents. The anthelmentic activity studies are performed using Indian earth worms. For this, the concentrated extract is diluted to various concentrations, and the effect of each solution is studied by measuring the time taken for paralysis and death of the earth worms. It is found to show significant anthelmentic activity at various concentrations compared with that of the standard drug Metronidazole.

  5. Speciated isotope dilution analysis of Cr(III) and Cr(VI) in water by ICP-DRC-MS. (United States)

    Ma, H-L; Tanner, P A


    An isotope dilution method has been developed for the speciation analysis of chromium in natural waters which accounts for species interconversions without the requirement of a separation instrument connected to the mass spectrometer. The method involves (i) in-situ spiking of the sample with isotopically enriched chromium species; (ii) separation of chromium species by precipitation with iron hydroxide; (iii) careful measurement of isotope ratios using an inductively coupled plasma mass spectrometer (ICP-MS) with a dynamic reaction cell (DRC) to remove isobaric polyatomic interferences. The method detection limits are 0.4 microg L(-1) for Cr(III) and 0.04 microg L(-1) for Cr(VI). The method is demonstrated for the speciation of Cr(III) and Cr(VI) in local nullah and synthetically spiked water samples. The percentage of conversion from Cr(III) to Cr(VI) increased from 5.9% to 9.3% with increase of the concentration of Cr(VI) and Cr(III) from 1 to 100 microg L(-1), while the reverse conversion from Cr(VI) to Cr(III) was observed within a range between 0.9% and 1.9%. The equilibrium constant for the conversion was found to be independent of the initial concentrations of Cr(III) and Cr(VI) and in the range of 1.0 (at pH 3) to 1.8 (at pH 10). The precision of the method is better than that of the DPC method for Cr(VI) analysis, with the added bonuses of freedom from interferences and simultaneous Cr(III) determination.

  6. Isotope Dilution - Thermal Ionisation Mass Spectrometric Analysis for Tin in a Fly Ash Material; Analisis de Estano en una Ceniza de Combustion mediante Espectrometria de Masas de Ionizacion Termica con Dilucion Isotopica

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez, C.; Fernandez, M.; Quejido, A. L.


    Isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) analysis has been applied to the determination of tin in a fly ash sample supplied by the EC Joint Research Centre (Ispra, Italy). The proposed procedure includes the silica gel/phosphoric acid technique for tin thermal ionisation activation and a strict heating protocol for isotope ratio measurements. Instrumental mass discrimination factor has been previously determined measuring a natural tin standard solution. Spike solutions has been prepared from 112Sn-enriched metal and quantified by reverse isotope dilution analysis. Two sample aliquots were spiked and tin was extracted with 4,5 M HCI during 25 min ultrasound exposure time. Due to the complex matrix of this fly ash material, a two-step purification stage using ion-exchange chromatography was required prior TIMS analysis. Obtained results for the two sample-spike blends (10,10 + - 0,55 y 10,50 + - 0,64 imolg-1) are comprarable, both value and uncertainty. Also a good reproducibility is observed between measurements. The proposed ID-TIMS procedure, as a primary method and due to the lack of fly ash reference material certified for tin content, can be used to validate more routine methodologies applied to tin determination in this kind of materials. (Author) 75 refs.

  7. Isotope dilution-GC-MS/MS analysis of 16 polycyclic aromatic hydrocarbons in selected medicinal herbs used as health food additives. (United States)

    Yu, L; Cao, Y; Zhang, J; Cui, Z; Sun, H


    Medicinal herbs have a very important role in health protection and disease control, and have been used in health foods. Polycyclic aromatic hydrocarbons (PAHs) have carcinogenic, biological and mutagenic effects. In this paper, the content of 16 PAHs as representative contaminants in nine Chinese medicinal herbs, as additives for health foods, was investigated in order to ensure food safety from this source. A highly sensitive isotope dilution-gas chromatography-tandem mass spectrometry (ID-GC-MS/MS) method combined with gel permeation chromatography (GPC) and solid-phase extraction (SPE) was developed. Calibration curves showed good linearity for all PAHs (R² > 0.999), and the limit of quantification (LOQ) ranged from 0.42 to 2.7 µg kg⁻¹. Average recoveries for these compounds were in the range of 52.5-117%, 52.6-119% and 81.4-108% at the concentrations of 10, 50 and 250 µg kg⁻¹ with RSD of 1.8-15%, 0.9-15% and 1.0-15%, respectively. The proposed method was used for the analysis of nine Chinese medicinal herbs. Total levels of PAHs varied from 98.2 µg kg⁻¹ (cassia seed) to 2245 µg kg⁻¹ (eucommia bark). The highest level was found for phenanthrene (Phe) in liquorice root (631.3 µg kg⁻¹), indigowoad leaf (551.0 µg kg⁻¹), rose flower (435.2 µg kg⁻¹) and eucommia bark (432.3 µg kg⁻¹). The proposed method could provide a useful basis for safety monitoring of herbs and risk management for PAHs in the health food industry.

  8. Quality- and dilution losses in the recycling of ferrous materials from end-of-life passenger cars: input-output analysis under explicit consideration of scrap quality. (United States)

    Nakamura, Shinichiro; Kondo, Yasushi; Matsubae, Kazuyo; Nakajima, Kenichi; Tasaki, Tomohiro; Nagasaka, Tetsuya


    Metals can in theory be infinitely recycled in a closed-loop without any degradation in quality. In reality, however, open-loop recycling is more typical for metal scrap recovered from end-of-life (EoL) products because mixing of different metal species results in scrap quality that no longer matches the originals. Further losses occur when meeting the quality requirement of the target product requires dilution of the secondary material by adding high purity materials. Standard LCA usually does not address these losses. This paper presents a novel approach to quantifying quality- and dilution losses, by means of hybrid input-output analysis. We focus on the losses associated with the recycling of ferrous materials from end-of-life vehicle (ELV) due to the mixing of copper, a typical contaminant in steel recycling. Given the quality of scrap in terms of copper density, the model determines the ratio by which scrap needs to be diluted in an electric arc furnace (EAF), and the amount of demand for EAF steel including those quantities needed for dilution. Application to a high-resolution Japanese IO table supplemented with data on ferrous materials including different grades of scrap indicates that a nationwide avoidance of these losses could result in a significant reduction of CO(2) emissions.

  9. Extraction and Analysis of Display Data (United States)

    Land, Chris; Moye, Kathryn


    The Display Audit Suite is an integrated package of software tools that partly automates the detection of Portable Computer System (PCS) Display errors. [PCS is a lap top computer used onboard the International Space Station (ISS).] The need for automation stems from the large quantity of PCS displays (6,000+, with 1,000,000+ lines of command and telemetry data). The Display Audit Suite includes data-extraction tools, automatic error detection tools, and database tools for generating analysis spread sheets. These spread sheets allow engineers to more easily identify many different kinds of possible errors. The Suite supports over 40 independent analyses, 16 NASA Tech Briefs, November 2008 and complements formal testing by being comprehensive (all displays can be checked) and by revealing errors that are difficult to detect via test. In addition, the Suite can be run early in the development cycle to find and correct errors in advance of testing.

  10. Web Template Extraction Based on Hyperlink Analysis

    Directory of Open Access Journals (Sweden)

    Julián Alarte


    Full Text Available Web templates are one of the main development resources for website engineers. Templates allow them to increase productivity by plugin content into already formatted and prepared pagelets. For the final user templates are also useful, because they provide uniformity and a common look and feel for all webpages. However, from the point of view of crawlers and indexers, templates are an important problem, because templates usually contain irrelevant information such as advertisements, menus, and banners. Processing and storing this information is likely to lead to a waste of resources (storage space, bandwidth, etc.. It has been measured that templates represent between 40% and 50% of data on the Web. Therefore, identifying templates is essential for indexing tasks. In this work we propose a novel method for automatic template extraction that is based on similarity analysis between the DOM trees of a collection of webpages that are detected using menus information. Our implementation and experiments demonstrate the usefulness of the technique.

  11. Improving oral bioavailability of metformin hydrochloride using water-in-oil microemulsions and analysis of phase behavior after dilution. (United States)

    Li, Yuan; Song, Jiaqi; Tian, Ning; Cai, Jie; Huang, Meihong; Xing, Qiao; Wang, Yalong; Wu, Chuanbin; Hu, Haiyan


    Microemulsions show significant promise for enhancing the oral bioavailability of biopharmaceutics classification system (BCS) class II drugs, but how about class III drugs remains unclear. Here we employed metformin hydrochloride (MET) as the model drug and prepared drug-loaded water-in-oil (W/O) microemulsions selecting different hydrophile-lipophile balance (HLB) surfactant systems, using HLB 8 as a cut-off. We examined the phase behaviors of microemulsions after dilution and attempted to correlate these behaviors to drug oral bioavailability. ME-A, including a lower content of surfactants (35%), underwent a transition of W/O emulsion and then became a stable O/W emulsion in a light milky appearance; ME-B, in contrast, introducing a higher content of surfactants (45%), still remained transparent or semitransparent upon dilution. Unexpectedly, ME-A showed significantly higher oral bioavailability, which can be reduced by blocking the lymphatic absorption pathway. Comparatively, the AUC of ME-B is lower, close to MET solution. Both microemulsions behaved similarly in intestinal perfusion test because of the dilution before perfusion, lacking of the important phase transition of W/O emulsion. These findings suggest that W/O microemulsions improve oral bioavailability of BCS class III drug by promoting lymphatic absorption. Analyzing the phase behavior of microemulsions after dilution may help predict the drug oral bioavailability and optimize formulations.

  12. Antibiogram and GC analysis of Euphorbia hirta leaf extract



    The antibiogram activity of ethanolic and aqueous extract of E.hirta was studied. Ethanol extract of the plant showed the maximal antibacterial activity and G.C Analysis showed the presence of citronellal. The extract showed inhibited the growth of E.coli, S.aureus, P.aeruginosa, Proteus etc.,

  13. An Object Extraction Model Using Association Rules and Dependence Analysis

    Institute of Scientific and Technical Information of China (English)


    Extracting objects from legacy systems is a basic step insystem's obje ct-orientation to improve the maintainability and understandability of the syst e ms. A new object extraction model using association rules an d dependence analysis is proposed. In this model data are classified by associat ion rules and the corresponding operations are partitioned by dependence analysis.

  14. The methodology of semantic analysis for extracting physical effects (United States)

    Fomenkova, M. A.; Kamaev, V. A.; Korobkin, D. M.; Fomenkov, S. A.


    The paper represents new methodology of semantic analysis for physical effects extracting. This methodology is based on the Tuzov ontology that formally describes the Russian language. In this paper, semantic patterns were described to extract structural physical information in the form of physical effects. A new algorithm of text analysis was described.

  15. Food Fish Identification from DNA Extraction through Sequence Analysis (United States)

    Hallen-Adams, Heather E.


    This experiment exposed 3rd and 4th y undergraduates and graduate students taking a course in advanced food analysis to DNA extraction, polymerase chain reaction (PCR), and DNA sequence analysis. Students provided their own fish sample, purchased from local grocery stores, and the class as a whole extracted DNA, which was then subjected to PCR,…

  16. Food Fish Identification from DNA Extraction through Sequence Analysis (United States)

    Hallen-Adams, Heather E.


    This experiment exposed 3rd and 4th y undergraduates and graduate students taking a course in advanced food analysis to DNA extraction, polymerase chain reaction (PCR), and DNA sequence analysis. Students provided their own fish sample, purchased from local grocery stores, and the class as a whole extracted DNA, which was then subjected to PCR,…

  17. Simultaneous analysis of oxybutynin and its active metabolite N-desethyl oxybutynin in human plasma by stable isotope dilution LC-MS/MS to support a bioequivalence study. (United States)

    Sharma, Primal; Patel, Daxesh P; Sanyal, Mallika; Berawala, Hiren; Guttikar, Swati; Shrivastav, Pranav S


    An isotope dilution high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed for the simultaneous determination of oxybutynin and its pharmacologically active metabolite N-desethyl oxybutynin in human plasma. Extraction of oxybutynin, its metabolite and their deuterated analogs as internal standards (ISs) from 300 μL human plasma was carried out by liquid-liquid extraction with methyl tert-butyl ether-ethyl acetate solvent mixture. Chromatographic separation of analytes was performed on Cosmosil C18 (150 mm × 4.6 mm, 5 μm) column under isocratic conditions with acetonitrile-1.0mM ammonium acetate (90:10, v/v) as the mobile phase. Six endogenous plasma phospholipids (496.3/184.0, 524.3/184.0, 758.5/184.0, 786.5/184.0, 806.5/184.0 and 810.5/184.0) were monitored to determine the extraction efficiency under different extraction conditions. The precursor→product ion transition for both the analytes and ISs were monitored on a triple quadrupole mass spectrometer, operating in the multiple reaction monitoring and positive ionization mode. The method was validated over a concentration range of 0.050-10.0 ng/mL for oxybutynin and 0.500-100 ng/mL for N-desethyl oxybutynin. The mean extraction recovery for analytes (80.4%) and ISs (76.9%) was consistent across five QC levels. Bench top, wet and dry extract, freeze-thaw and long term stability was evaluated for both the analytes. The method was applied to support a bioequivalence study of 5mg tablet formulation in 74 healthy Indian subjects. Assay reproducibility was demonstrated by reanalysis of 344 incurred samples.

  18. Extracting Minerals from Seawater: An Energy Analysis

    Directory of Open Access Journals (Sweden)

    Ugo Bardi


    Full Text Available The concept of recovering minerals from seawater has been proposed as a way of counteracting the gradual depletion of conventional mineral ores. Seawater contains large amounts of dissolved ions and the four most concentrated metal ones (Na, Mg, Ca, K are being commercially extracted today. However, all the other metal ions exist at much lower concentrations. This paper reports an estimate of the feasibility of the extraction of these metal ions on the basis of the energy needed. In most cases, the result is that extraction in amounts comparable to the present production from land mines would be impossible because of the very large amount of energy needed. This conclusion holds also for uranium as fuel for the present generation of nuclear fission plants. Nevertheless, in a few cases, mainly lithium, extraction from seawater could provide amounts of metals sufficient for closing the cycle of metal use in the economy, provided that an increased level of recycling can be attained.

  19. Isotope dilution gas chromatography with mass spectrometry for the analysis of 4-octyl phenol, 4-nonylphenol, and bisphenol A in vegetable oils. (United States)

    Wu, Pinggu; Zhang, Liqun; Yang, Dajin; Zhang, Jing; Hu, Zhengyan; Wang, Liyuan; Ma, Bingjie


    By the combination of solid-phase extraction as well as isotope dilution gas chromatography with mass spectrometry, a sensitive and reliable method for the determination of endocrine-disrupting chemicals including bisphenol A, 4-octylphenol, and 4-nonylphenol in vegetable oils was established. The application of a silica/N-(n-propyl)ethylenediamine mixed solid-phase extraction cartridge achieved relatively low matrix effects for bisphenol A, 4-octylphenol, and 4-nonylphenol in vegetable oils. Experiments were designed to evaluate the effects of derivatization, and the extraction parameters were optimized. The estimated limits of detection and quantification for bisphenol A, 4-octylphenol, and 4-nonylphenol were 0.83 and 2.5 μg/kg, respectively. In a spiked experiment in vegetable oils, the recovery of the added bisphenol A was 97.5-110.3%, recovery of the added 4-octylphenol was 64.4-87.4%, and that of 4-nonylphenol was 68.2-89.3%. This sensitive method was then applied to real vegetable oil samples from Zhejiang Province of China, and none of the target compounds were detected.

  20. Development of pitanga nectar with different sweeteners by sensory analysis: ideal pulp dilution, ideal sweetness, and sweetness equivalence

    Directory of Open Access Journals (Sweden)

    Mírian Luisa Faria Freitas


    Full Text Available The objective of this study was to develop pitanga nectar formulations in which sucrose was replaced with different sweeteners. Consumer tests were conducted with 50 fruit juice consumers, and a just-about-right scale was used to determine the ideal pulp dilution and ideal sweetness with sucrose. Furthermore, the adequate concentrations of six sweeteners were determined to obtain the equivalent sweetness of sucrose using relative to these concentrations the magnitude estimation model with 19 selected assessors. The ideal dilution test resulted in 25% pulp, and the ideal sweetness test, 10% sucrose. Sweetener concentrations to replace sucrose were 0.0160%, 0.0541%, 0.1000%, 0.0999%, 0.0017%, and 0.0360%, respectively, for sucralose, aspartame, stevia 40% rebaudioside A, stevia 95% rebaudioside A, neotame, and a 2:1 cyclamate/saccharin blend. These results can be used to prepare pitanga nectar with different sweeteners and obtain the same sweetness intensity in less caloric products than that of nectar prepared with sucrose.

  1. Electromembrane extraction for pharmaceutical and biomedical analysis

    DEFF Research Database (Denmark)

    Huang, Chuixiu; Seip, Knut Fredrik; Gjelstad, Astrid


    Electromembrane extraction (EME) was presented as a new microextraction concept in 2006, and since the introduction, substantial research has been conducted to develop this concept in different areas of analytical chemistry. To date, more than 100 research papers have been published on EME...

  2. Pore-scale analysis on the effects of compound-specific dilution on transient transport and solute breakthrough

    DEFF Research Database (Denmark)

    Rolle, Massimo; Kitanidis, Peter

    Compound-specific diffusivities significantly impact solute transport and mixing at different scales. Although diffusive processes occur at the small pore scale, their effects propagate and remain important at larger macroscopic scales [1]. In this pore-scale modeling study in saturated porous...... media we show that compound-specific effects are important not only at steady-state and for the lateral displacement of solutes with different diffusivities but also for transient transport and solute breakthrough [2]. We performed flow and transport simulations in two-dimensional pore-scale domains...... significant effects of aqueous diffusion on solute breakthrough curves. However, the magnitude of such effects can be masked by the flux-averaging approach used to measure solute breakthrough and can hinder the correct interpretation of the true dilution of different solutes. We propose, as a metric of mixing...

  3. Cavitation pulse extraction and centrifugal pump analysis

    Energy Technology Data Exchange (ETDEWEB)

    Luo, Hong Lind Shaoran [University of Electronic Science and Technology of China, Chengdu (China); Yu, Bo; Qing, Biao [Xihua University, Chengdu (China)


    This study extracted cavitation pulses from hydrophone signals sampled in a centrifugal pump and analyzed their characteristics. The modified and simplified Empirical mode decomposition (EMD) algorithm was proposed for extracting cavitation pulses from strong background noise. Experimental results showed that EMD can effectively suppress noise and obtain clear cavitation pulses, facilitating the identification of the number of pulses associated with the degree of cavitation. The cavitation characteristics were modeled to predict the value of incipient cavitation. Then, we proposed a method for detecting the wear of the impeller surface. That is, the information on the impeller surface of the centrifugal pump, including the roughness of the impeller surface and its wear trends, were quantified based on the net positive suction head available of incipient cavitation. The findings indicate that the proposed technique is suitable for condition monitoring of the pump.

  4. Biochemical analysis of extracting fermented coconut oil



    Vegetable oil can be produced from a perennial plant such as coconut (Cocos nucifera L.). There are few techniques for coconut oil extraction, such as physical, chemical, and fermentative processes. The fermentation process uses microbial inoculum as starter. Ground coconut meat was soaked in warm water, than squeezed several times to get coconut milk. After being allowed to stand for 4-5 hours, it separated into two layers, cream and skim. Starter was prepared from a mixture of milk and coco...

  5. Linguistic feature analysis for protein interaction extraction

    Directory of Open Access Journals (Sweden)

    Cornelis Chris


    Full Text Available Abstract Background The rapid growth of the amount of publicly available reports on biomedical experimental results has recently caused a boost of text mining approaches for protein interaction extraction. Most approaches rely implicitly or explicitly on linguistic, i.e., lexical and syntactic, data extracted from text. However, only few attempts have been made to evaluate the contribution of the different feature types. In this work, we contribute to this evaluation by studying the relative importance of deep syntactic features, i.e., grammatical relations, shallow syntactic features (part-of-speech information and lexical features. For this purpose, we use a recently proposed approach that uses support vector machines with structured kernels. Results Our results reveal that the contribution of the different feature types varies for the different data sets on which the experiments were conducted. The smaller the training corpus compared to the test data, the more important the role of grammatical relations becomes. Moreover, deep syntactic information based classifiers prove to be more robust on heterogeneous texts where no or only limited common vocabulary is shared. Conclusion Our findings suggest that grammatical relations play an important role in the interaction extraction task. Moreover, the net advantage of adding lexical and shallow syntactic features is small related to the number of added features. This implies that efficient classifiers can be built by using only a small fraction of the features that are typically being used in recent approaches.

  6. Biochemical analysis of extracting fermented coconut oil

    Directory of Open Access Journals (Sweden)



    Full Text Available Vegetable oil can be produced from a perennial plant such as coconut (Cocos nucifera L.. There are few techniques for coconut oil extraction, such as physical, chemical, and fermentative processes. The fermentation process uses microbial inoculum as starter. Ground coconut meat was soaked in warm water, than squeezed several times to get coconut milk. After being allowed to stand for 4-5 hours, it separated into two layers, cream and skim. Starter was prepared from a mixture of milk and coconut water (1:9, v/v which enriched with 2% tomato extract, 0.5% urea, and 1.0% molasses and then preincubated for 5 days under agitation. Starter with different concentration (1.0; 2.5; 5.0; and 10% were added onto coconut milk and allowed to be fermented for over night. The extracting oil was analyzed for further experiment, especially, on its antibacterial activity. The maximum yield of 23% was achieved by using 2.5% starter. Total protein, fat, FFA, and cholesterol content of the fermented coconut oil were 0.05%, 96.45%, 0.29%, and 0.008%, respectively. The gas chromatogram showed that this oil contained high lauric acid (46.20%, and 13.94% miristic, 5.97% palmitic, 9.00% palmitoleic, and 19.73% stearic acid, respectively.

  7. Watermark Detection and Extraction Using Independent Component Analysis Method

    Directory of Open Access Journals (Sweden)

    Yu Dan


    Full Text Available This paper proposes a new image watermarking technique, which adopts Independent Component Analysis (ICA for watermark detection and extraction process (i.e., dewatermarking. Watermark embedding is performed in the spatial domain of the original image. Watermark can be successfully detected during the Principle Component Analysis (PCA whitening stage. A nonlinear robust batch ICA algorithm, which is able to efficiently extract various temporally correlated sources from their observed linear mixtures, is used for blind watermark extraction. The evaluations illustrate the validity and good performance of the proposed watermark detection and extraction scheme based on ICA. The accuracy of watermark extraction depends on the statistical independence between the original, key and watermark images and the temporal correlation of these sources. Experimental results demonstrate that the proposed system is robust to several important image processing attacks, including some geometrical transformations—scaling, cropping and rotation, quantization, additive noise, low pass filtering, multiple marks, and collusion.

  8. Building Extraction from LIDAR Based Semantic Analysis

    Institute of Scientific and Technical Information of China (English)

    YU Jie; YANG Haiquan; TAN Ming; ZHANG Guoning


    Extraction of buildings from LIDAR data has been an active research field in recent years. A scheme for building detection and reconstruction from LIDAR data is presented with an object-oriented method which is based on the buildings' semantic rules. Two key steps are discussed: how to group the discrete LIDAR points into single objects and how to establish the buildings' semantic rules. In the end, the buildings are reconstructed in 3D form and three common parametric building models (flat, gabled, hipped) are implemented.

  9. Extraction and Analysis of Terpenes/Terpenoids. (United States)

    Jiang, Zuodong; Kempinski, Chase; Chappell, Joe


    Terpenes/terpenoids constitute one of the largest classes of natural products, this is due to the incredible chemical diversity that can arise from the biochemical transformations of the relatively simple prenyl diphosphate starter units. All terpenes/terpenoids comprise a hydrocarbon backbone that is generated from the various length prenyl diphosphates (a polymer chain of prenyl units). Upon ionization (removal) of the diphosphate group, the remaining allylic carbocation intermediates can be coaxed down complex chemical cascades leading to diverse linear and cyclized hydrocarbon backbones, which can then be further modified with a wide range of functional groups (e.g. alcohol, ketones, etc.) and substituent additions (e.g. sugars, fatty acids). Because of this chemical diversity, terpenes/terpenoids have great industrial uses as flavors, fragrances, high grade lubricants, biofuels, agricultural chemicals and medicines. The protocols presented here focus on the extraction of terpenes/terpenoids from various plant sources and have been divided into extraction methods for terpenes/terpenoids with various levels of chemical decoration, from the relative small, nonpolar, volatile hydrocarbons to substantially large molecules with greater physical complexity due to their chemical modifications.

  10. Stochastic empirical loading and dilution model for analysis of flows, concentrations, and loads of highway runoff constituents (United States)

    Granato, Gregory E.; Jones, Susan C.


    In cooperation with FHWA, the U.S. Geological Survey developed the stochastic empirical loading and dilution model (SELDM) to supersede the 1990 FHWA runoff quality model. The SELDM tool is designed to transform disparate and complex scientific data into meaningful information about the adverse risks of runoff on receiving waters, the potential need for mitigation measures, and the potential effectiveness of such measures for reducing such risks. The SELDM tool is easy to use because much of the information and data needed to run it are embedded in the model and obtained by defining the site location and five simple basin properties. Information and data from thousands of sites across the country were compiled to facilitate the use of the SELDM tool. A case study illustrates how to use the SELDM tool for conducting the types of sensitivity analyses needed to properly assess water quality risks. For example, the use of deterministic values to model upstream stormflows instead of representative variations in prestorm flow and runoff may substantially overestimate the proportion of highway runoff in downstream flows. Also, the risks for total phosphorus excursions are substantially affected by the selected criteria and the modeling methods used. For example, if a single deterministic concentration is used rather than a stochastic population of values to model upstream concentrations, then the percentage of water quality excursions in the downstream receiving waters may depend entirely on the selected upstream concentration.

  11. Qualitative analysis of hexane flour extract of spelt

    Directory of Open Access Journals (Sweden)

    Vujić Đura N.


    Full Text Available Gas chromatography with mass spectrometry (GC-MS was used for performing a qualitative analysis of the hexane flour extract of three samples of spelt. All the three samples were first treated with hexane and the obtained extracts were used for the analysis of the fatty acid lipid components. The transesterification reaction was performed using TMSH (trimethylsulfonium hydroxide, 0.2M in methanol, and the fatty acids were esterified from acylglycerol to methyl-esters. In all analyzed extracts, the predominant component was methyl linoleate, followed by methyl oleate and methyl palmitate. The subsequent tests, performed by cluster analysis, were used to compare the hexane flour extracts of different types of spelt. [Projekat Ministarstva nauke Republike Srbije, br. III46005 i br. TR 31066

  12. Estimating the extractability of potentially toxic metals in urban soils: A comparison of several extracting solutions

    Energy Technology Data Exchange (ETDEWEB)

    Madrid, F. [Instituto de Recursos Naturales y Agrobiologia de Sevilla (CSIC), Apartado 1052, 41080 Sevilla (Spain); Reinoso, R. [Instituto de Recursos Naturales y Agrobiologia de Sevilla (CSIC), Apartado 1052, 41080 Sevilla (Spain); Florido, M.C. [Departamento de Cristalografia, Mineralogia y Quimica Agricola, Universidad de Sevilla, Avda. Reina Mercedes, s/n, 41012 Sevilla (Spain); Diaz Barrientos, E. [Instituto de Recursos Naturales y Agrobiologia de Sevilla (CSIC), Apartado 1052, 41080 Sevilla (Spain); Ajmone-Marsan, F. [DI.VA.P.R.A., Chimica Agraria, Universita di Torino, Via Leonardo da Vinci, 44, 10095 Grugliasco, Torino (Italy); Davidson, C.M. [Department of Pure and Applied Chemistry, University of Strathclyde, 295 Cathedral Street, Glasgow G1 1XL, Scotland (United Kingdom); Madrid, L. [Instituto de Recursos Naturales y Agrobiologia de Sevilla (CSIC), Apartado 1052, 41080 Sevilla (Spain)]. E-mail:


    Metals released by the extraction with aqua regia, EDTA, dilute HCl and sequential extraction (SE) by the BCR protocol were studied in urban soils of Sevilla, Torino, and Glasgow. By multivariate analysis, the amounts of Cu, Pb and Zn liberated by any method were statistically associated with one another, whereas other metals were not. The mean amounts of all metals extracted by HCl and by SE were well correlated, but SE was clearly underestimated by HCl. Individual data for Cu, Pb and Zn by both methods were correlated only if each city was considered separately. Other metals gave poorer relationships. Similar conclusions were reached comparing EDTA and HCl, with much lower values for EDTA. Dilute HCl extraction cannot thus be recommended for general use as alternative to BCR SE in urban soils. - Dilute HCl extraction is tested as an alternative to the BCR sequential extraction in urban soils.

  13. Sono-assisted extraction of alcohol-insoluble extract from Althaea rosea: purification and chemical analysis. (United States)

    Eskandari, Meghdad; Samavati, Vahid


    A Box-Behnken design (BBD) was used to evaluate the effects of ultrasonic power, extraction time, extraction temperature, and water to raw material ratio on extraction yield of alcohol-insoluble polysaccharide of Althaea rosea leaf (ARLP). Purification was carried out by dialysis method. Chemical analysis of ARLP revealed contained 12.69 ± 0.48% moisture, 79.33 ± 0.51% total sugar, 3.82 ± 0.21% protein, 11.25 ± 0.37% uronic acid and 3.77 ± 0.15% ash. The response surface methodology (RSM) showed that the significant quadratic regression equation with high R(2) (=0.9997) was successfully fitted for extraction yield of ARLP as function of independent variables. The overall optimum region was found to be at the combined level of ultrasonic power 91.85 W, extraction time 29.94 min, extraction temperature 89.78 °C, and the ratio of water to raw material 28.77 (mL/g). At this optimum point, extraction yield of ARLP was 19.47 ± 0.41%. No significant (p>0.05) difference was found between the actual and predicted (19.30 ± 0.075%) values. The results demonstrated that ARLP had strong scavenging activities on DPPH and hydroxyl radicals.

  14. Analysis of magnetic mechanisms of 3d-doped ZnO diluted magnetic semiconductors by an abnormal peak on M-T curve

    Institute of Scientific and Technical Information of China (English)


    The crystallographic structures and magnetic properties of a Zn0.95Co0.05O thin film deposited on a C-sapphire substrate using a dual-beam pulsed laser deposition method were characterized. It was shown from crystallographic analysis that the film belongs to the wurtzite structure with the C-axis aligned with that of the substrate. Magnetic hysteresis loops were observed till up to room temperature. A small peak around 55 K was noticed on the magnetization vs. temperature curve. The corresponding temperature of the small peak is close to that of 'the abnormal peak' reported by X.M. Zhang et al. From the results obtained, no correlation was found between the abnormal peak and the quantum effects. The magnetic behaviors in the Zn0.95Co0.05O film cannot be explained by the ferromagnetism in diluted magnetic semiconductors. The magnetic mechanisms in ZnO-based diluted magnetic semiconductors are also discussed.

  15. Analysis of near-infrared spectroscopy and indocyanine green dye dilution with Monte Carlo simulation of light propagation in the adult brain (United States)

    Mudra, Regina M.; Nadler, Andreas; Keller, Emanuela; Niederer, Peter F.


    Near-infrared spectroscopy (NIRS) combined with indocyanine green (ICG) dilution is applied externally on the head to determine the cerebral hemodynamics of neurointensive care patients. We applied Monte Carlo simulation for the analysis of a number of problems associated with this method. First, the contamination of the optical density (OD) signal due to the extracerebral tissue was assessed. Second, the measured OD signal depends essentially on the relative blood content (with respect to its absorption) in the various transilluminated tissues. To take this into account, we weighted the calculated densities of the photon distribution under baseline conditions within the different tissues with the changes and aberration of the relative blood volumes that are typically observed under healthy and pathologic conditions. Third, in case of NIRS ICG dye dilution, an ICG bolus replaces part of the blood such that a transient change of absorption in the brain tissues occurs that can be recorded in the OD signal. Our results indicate that for an exchange fraction of Δ=30% of the relative blood volume within the intracerebral tissue, the OD signal is determined from 64 to 74% by the gray matter and between 8 to 16% by the white matter maximally for a distance of d=4.5 cm.

  16. Hybridizing pines with diluted pollen (United States)

    Robert Z. Callaham


    Diluted pollens would have many uses by the tree breeder. Dilutions would be particularly advantageous in making many controlled pollinations with a limited amount of pollen. They also would be useful in artificial mass pollinations of orchards or single trees. Diluted pollens might help overcome troublesome genetic barriers to crossing. Feasibility o,f using diluted...

  17. Analysis of Platelet-Rich Plasma Extraction (United States)

    Fitzpatrick, Jane; Bulsara, Max K.; McCrory, Paul Robert; Richardson, Martin D.; Zheng, Ming Hao


    Background: Platelet-rich plasma (PRP) has been extensively used as a treatment in tissue healing in tendinopathy, muscle injury, and osteoarthritis. However, there is variation in methods of extraction, and this produces different types of PRP. Purpose: To determine the composition of PRP obtained from 4 commercial separation kits, which would allow assessment of current classification systems used in cross-study comparisons. Study Design: Controlled laboratory study. Methods: Three normal adults each donated 181 mL of whole blood, some of which served as a control and the remainder of which was processed through 4 PRP separation kits: GPS III (Biomet Biologics), Smart-Prep2 (Harvest Terumo), Magellan (Arteriocyte Medical Systems), and ACP (Device Technologies). The resultant PRP was tested for platelet count, red blood cell count, and white blood cell count, including differential in a commercial pathology laboratory. Glucose and pH measurements were obtained from a blood gas autoanalyzer machine. Results: Three kits taking samples from the “buffy coat layer” were found to have greater concentrations of platelets (3-6 times baseline), while 1 kit taking samples from plasma was found to have platelet concentrations of only 1.5 times baseline. The same 3 kits produced an increased concentration of white blood cells (3-6 times baseline); these consisted of neutrophils, leukocytes, and monocytes. This represents high concentrations of platelets and white blood cells. A small drop in pH was thought to relate to the citrate used in the sample preparation. Interestingly, an unexpected increase in glucose concentrations, with 3 to 6 times greater than baseline levels, was found in all samples. Conclusion: This study reveals the variation of blood components, including platelets, red blood cells, leukocytes, pH, and glucose in PRP extractions. The high concentrations of cells are important, as the white blood cell count in PRP samples has frequently been ignored

  18. Determination of water-soluble and insoluble (dilute-HCl-extractable) fractions of Cd, Pb and Cu in Antarctic aerosol by square wave anodic stripping voltammetry: distribution and summer seasonal evolution at Terra Nova Bay (Victoria Land)

    Energy Technology Data Exchange (ETDEWEB)

    Annibaldi, A.; Truzzi, C.; Illuminati, S.; Bassotti, E.; Scarponi, G. [Polytechnic University of Marche - Ancona, Department of Marine Science, Ancona (Italy)


    Eight PM10 aerosol samples were collected in the vicinity of the ''Mario Zucchelli'' Italian Antarctic Station (formerly Terra Nova Bay Station) during the 2000-2001 austral summer using a high-volume sampler and precleaned cellulose filters. The aerosol mass was determined by differential weighing of filters carried out in a clean chemistry laboratory under controlled temperature and humidity. A two-step sequential extraction procedure was used to separate the water-soluble and the insoluble (dilute-HCl-extractable) fractions. Cd, Pb and Cu were determined in the two fractions using an ultrasensitive square wave anodic stripping voltammetric (SWASV) procedure set up for and applied to aerosol samples for the first time. Total extractable metals showed maxima at midsummer for Cd and Pb and a less clear trend for Cu. In particular, particulate metal concentrations ranged as follows: Cd 0.84-9.2 {mu}g g{sup -1} (average 4.7 {mu}g g{sup -1}), Pb 13.2-81 {mu}g g{sup -1} (average 33 {mu}g g{sup -1}), Cu 126-628 {mu}g g{sup -1} (average 378 {mu}g g{sup -1}). In terms of atmospheric concentration, the values were: Cd 0.55-6.3 pg m{sup -3} (average 3.4 pg m{sup -3}), Pb 8.7-48 pg m{sup -3} (average 24 pg m{sup -3}), Cu 75-365 pg m{sup -3} (average 266 pg m{sup -3}). At the beginning of the season the three metals appear widely distributed in the insoluble (HCl-extractable) fraction (higher proportions for Cd and Pb, 90-100%, and lower for Cu, 70-90%) with maxima in the second half of December. The soluble fraction then increases, and at the end of the season Cd and Pb are approximately equidistributed between the two fractions, while for Cu the soluble fraction reaches its maximum level of 36%. Practically negligible contributions are estimated for crustal and sea-spray sources. Low but significant volcanic contributions are estimated for Cd and Pb ({proportional_to}10% and {proportional_to}5%, respectively), while there is an evident although not

  19. The Stylistic Analysis of an Extract from The Rainbow

    Institute of Scientific and Technical Information of China (English)



      This paper makes a detailed stylistic analysis of an extract from The Rainbow by Lawrence based on lexical features, grammatical features and figure of speech. Through the analysis, a better aesthetic appreciation and deeper understanding of the novel will be achieved.

  20. Solid-phase extraction procedures in systematic toxicological analysis

    NARCIS (Netherlands)

    Franke, J.P.; de Zeeuw, R.A


    In systematic toxicological analysis (STA) the substance(s) present is (are) not known at the start of the analysis. in such an undirected search the extraction procedure cannot be directed to a given substance but must be a general procedure where a compromise must be reached in that the substances

  1. Retinal image analysis: preprocessing and feature extraction

    Energy Technology Data Exchange (ETDEWEB)

    Marrugo, Andres G; Millan, Maria S, E-mail: [Grup d' Optica Aplicada i Processament d' Imatge, Departament d' Optica i Optometria Univesitat Politecnica de Catalunya (Spain)


    Image processing, analysis and computer vision techniques are found today in all fields of medical science. These techniques are especially relevant to modern ophthalmology, a field heavily dependent on visual data. Retinal images are widely used for diagnostic purposes by ophthalmologists. However, these images often need visual enhancement prior to apply a digital analysis for pathological risk or damage detection. In this work we propose the use of an image enhancement technique for the compensation of non-uniform contrast and luminosity distribution in retinal images. We also explore optic nerve head segmentation by means of color mathematical morphology and the use of active contours.

  2. Use of isotope-labeled aflatoxins for LC-MS/MS stable isotope dilution analysis of foods. (United States)

    Cervino, Christian; Asam, Stefan; Knopp, Dietmar; Rychlik, Michael; Niessner, Reinhard


    Aflatoxins are a group of very carcinogenic mycotoxins that can be found on a wide range of food commodities including nuts, cereals, and spices. In this study, the first LC-MS/MS stable isotope dilution assay (SIDA) for the determination of aflatoxins in foods was developed. The development of this method was enabled by easily accessible isotope-labeled (deuterated) aflatoxins B2 and G2, which were synthesized by catalytic deuteration of aflatoxin B1 and G1, purified, and well-characterized by NMR and MS. All four aflatoxins of interest (B1, B2, G1, and G2) were quantified in food samples by using these two labeled internal standards. The response factors (RF) of the linear calibrations were revealed to be matrix independent for labeled aflatoxin B2/aflatoxin B2 and labeled aflatoxin G2/aflatoxin G2. For labeled aflatoxin B 2/aflatoxin B 1 and labeled aflatoxin B2/aflatoxin G1 matrix-matched calibration was performed for the model matrices almonds and wheat flour, showing significant differences of the RFs. Limits of detection (LOD) were determined by applying a statistical approach in the presence of the two model matrices, yielding 0.31 microg/kg (aflatoxin B1), 0.09 microg/kg (aflatoxin B2), 0.38 microg/kg (aflatoxin G1), and 0.32 microg/kg (aflatoxin G2) for almonds (similar LODs were obtained for wheat flour). Recovery rates were between 90 and 105% for all analytes. Coefficients of variation (CV) of 12% (aflatoxin B1), 3.6% (aflatoxin B2), 14% (aflatoxin G1), and 4.8% (aflatoxin G2) were obtained from interassay studies. For further validation, a NIST standard reference food sample was analyzed for aflatoxins B1 and B2. The method was successfully applied to determine trace levels of aflatoxins in diverse food matrices such as peanuts, nuts, grains, and spices. Aflatoxin contents in these samples ranged from about 0.5 to 6 microg/kg.

  3. The connection analysis between the dilution of the deposited Fe-Cr-V-Mo-C layer by the basic metal and the parameters of its microstructure (United States)

    Degterev, A. S.; Gnusov, S. F.


    In this work, the structure of the Fe-Cr-V-Mo-C coatings received by plasma transferred arc cladding was investigated. Coatings were deposited on plates with a thickness of 10 mm and made from constructional steel (steel 20). The correlation analysis of relationships between dilution of the deposited layers by the basic metal and the parameters of their microstructure was carried out. The parameters were as follows: volume fraction, a size, a shape factor, the distance between particles, the number of particles of vanadium carbide, volume fraction of the eutectic on the basis of carbide M7C3 and the distances between its colonies, as well as the volume fraction of the α-phase in the alloy matrix.

  4. Smart Extraction and Analysis System for Clinical Research. (United States)

    Afzal, Muhammad; Hussain, Maqbool; Khan, Wajahat Ali; Ali, Taqdir; Jamshed, Arif; Lee, Sungyoung


    With the increasing use of electronic health records (EHRs), there is a growing need to expand the utilization of EHR data to support clinical research. The key challenge in achieving this goal is the unavailability of smart systems and methods to overcome the issue of data preparation, structuring, and sharing for smooth clinical research. We developed a robust analysis system called the smart extraction and analysis system (SEAS) that consists of two subsystems: (1) the information extraction system (IES), for extracting information from clinical documents, and (2) the survival analysis system (SAS), for a descriptive and predictive analysis to compile the survival statistics and predict the future chance of survivability. The IES subsystem is based on a novel permutation-based pattern recognition method that extracts information from unstructured clinical documents. Similarly, the SAS subsystem is based on a classification and regression tree (CART)-based prediction model for survival analysis. SEAS is evaluated and validated on a real-world case study of head and neck cancer. The overall information extraction accuracy of the system for semistructured text is recorded at 99%, while that for unstructured text is 97%. Furthermore, the automated, unstructured information extraction has reduced the average time spent on manual data entry by 75%, without compromising the accuracy of the system. Moreover, around 88% of patients are found in a terminal or dead state for the highest clinical stage of disease (level IV). Similarly, there is an ∼36% probability of a patient being alive if at least one of the lifestyle risk factors was positive. We presented our work on the development of SEAS to replace costly and time-consuming manual methods with smart automatic extraction of information and survival prediction methods. SEAS has reduced the time and energy of human resources spent unnecessarily on manual tasks.

  5. Stable isotope dilution analysis of salicylic acid and hydroquinone in human skin samples by gas chromatography with mass spectrometric detection. (United States)

    Judefeind, Anja; van Rensburg, Peet Jansen; Langelaar, Stephan; du Plessis, Jeanetta


    A sensitive and accurate gas chromatographic-mass spectrometric (GC-MS) method has been developed for the quantitative determination of salicylic acid (SA) and hydroquinone (HQ) from human skin samples and cosmetic emulsions. Deuterium labeled SA-d(6) and HQ-d(6) were used as internal standards (IS). The samples were extracted with methanol, dried under nitrogen and derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)+1% trimethylchlorosilane (TMCS). Quantification was performed in SIM mode with a limit of quantification (LOQ) of 50 ng ml(-1) for SA and 10 ng ml(-1) for HQ. The inter-day variation (R.S.D.) was less than 5% and the accuracy was better than 13.3% for both compounds. The recoveries from the different matrices ranged between 93.1 and 103.3% for SA, and 97.3 and 100.8% for HQ.

  6. Order Parameters of the Dilute A Models

    CERN Document Server

    Warnaar, S O; Seaton, K A; Nienhuis, B


    The free energy and local height probabilities of the dilute A models with broken $\\Integer_2$ symmetry are calculated analytically using inversion and corner transfer matrix methods. These models possess four critical branches. The first two branches provide new realisations of the unitary minimal series and the other two branches give a direct product of this series with an Ising model. We identify the integrable perturbations which move the dilute A models away from the critical limit. Generalised order parameters are defined and their critical exponents extracted. The associated conformal weights are found to occur on the diagonal of the relevant Kac table. In an appropriate regime the dilute A$_3$ model lies in the universality class of the Ising model in a magnetic field. In this case we obtain the magnetic exponent $\\delta=15$ directly, without the use of scaling relations.

  7. Magnetic Solid Phase Extraction Applied to Food Analysis

    Directory of Open Access Journals (Sweden)

    Israel S. Ibarra


    Full Text Available Magnetic solid phase extraction has been used as pretreatment technique for the analysis of several compounds because of its advantages when it is compared with classic methods. This methodology is based on the use of magnetic solids as adsorbents for preconcentration of different analytes from complex matrices. Magnetic solid phase extraction minimizes the use of additional steps such as precipitation, centrifugation, and filtration which decreases the manipulation of the sample. In this review, we describe the main procedures used for synthesis, characterization, and application of this pretreatment technique which were applied in food analysis.

  8. A Procedure for the supercritical fluid extraction of coal samples, with subsequent analysis of extracted hydrocarbons (United States)

    Kolak, Jonathan J.


    Introduction: This report provides a detailed, step-by-step procedure for conducting extractions with supercritical carbon dioxide (CO2) using the ISCO SFX220 supercritical fluid extraction system. Protocols for the subsequent separation and analysis of extracted hydrocarbons are also included in this report. These procedures were developed under the auspices of the project 'Assessment of Geologic Reservoirs for Carbon Dioxide Sequestration' (see to investigate possible environmental ramifications associated with CO2 storage (sequestration) in geologic reservoirs, such as deep (~1 km below land surface) coal beds. Supercritical CO2 has been used previously to extract contaminants from geologic matrices. Pressure-temperature conditions within deep coal beds may render CO2 supercritical. In this context, the ability of supercritical CO2 to extract contaminants from geologic materials may serve to mobilize noxious compounds from coal, possibly complicating storage efforts. There currently exists little information on the physicochemical interactions between supercritical CO2 and coal in this setting. The procedures described herein were developed to improve the understanding of these interactions and provide insight into the fate of CO2 and contaminants during simulated CO2 injections.


    Directory of Open Access Journals (Sweden)

    Demyanenko DV


    Full Text Available The purpose of this work was to make qualitative and quantitative analysis of phenolic biologically active substances (BAS in the extracts produced from lime flowers with condensed gases, using method of high-performance liquid chromatography (HPLC. Materials and methods: materials for this study were the extracts obtained by consequent processing of the herbal drug and marcs thereof with various condensed gases: difluorochloromethane (Freon R22, difluoromethane (Freon R32, azeotropic mixture of difluoromethane with pentafluoroethane (Freon 410A and freon-ammonium mixture. Extracts obtained with the latter were subjected to further fractionation by liquidliquid separation into hexane, chloroform, ethyl acetate and aqueous-alcohol phases. Besides, the supercritical СО2 extract, obtained from the herbal drug under rather strong conditions (at temperature 60°С and pressure 400 bar, was studied in our previous research. Presence of phenolic BAS and their quantity in the researched samples were determined by method of HPLC with UVspectrometric detection. Results and discussion: It has been found that Freon R22 extracted trace amounts of rutin from lime flowers – its content was only 0.08% of the total extract weight. On the other hand, Freons R32 and R410А showed good selectivity to moderately polar BAS of lime flowers (derivatives of flavonoids and hydroxycinnamic acids: in particular, the extract obtained with freon R32 contained about 1.3% of the total phenolic substances, and it was the only one of the investigated condensed gases used by us which took the basic flavonoid of lime flowers tiliroside – its content was 0.42% of extract weight. Also Freons R32 and R410А were able to withdraw another compound dominating among phenolic substances in the yielded extracts. Its quantity was rather noticeable – up to 0.87% of extract weight. This substance was not identified by existing database, but its UV-spectrum was similar to those of

  10. Direct Sampling and Analysis from Solid Phase Extraction Cards using an Automated Liquid Extraction Surface Analysis Nanoelectrospray Mass Spectrometry System

    Energy Technology Data Exchange (ETDEWEB)

    Walworth, Matthew J [ORNL; ElNaggar, Mariam S [ORNL; Stankovich, Joseph J [ORNL; WitkowskiII, Charles E. [Protein Discovery, Inc.; Norris, Jeremy L [ORNL; Van Berkel, Gary J [ORNL


    Direct liquid extraction based surface sampling, a technique previously demonstrated with continuous flow and autonomous pipette liquid microjunction surface sampling probes, has recently been implemented as the Liquid Extraction Surface Analysis (LESA) mode on the commercially available Advion NanoMate chip-based infusion nanoelectrospray ionization system. In the present paper, the LESA mode was applied to the analysis of 96-well format custom solid phase extraction (SPE) cards, with each well consisting of either a 1 or 2 mm diameter monolithic hydrophobic stationary phase. These substrate wells were conditioned, loaded with either single or multi-component aqueous mixtures, and read out using the LESA mode of a TriVersa NanoMate or a Nanomate 100 coupled to an ABI/Sciex 4000QTRAPTM hybrid triple quadrupole/linear ion trap mass spectrometer and a Thermo LTQ XL linear ion trap mass spectrometer. Extraction conditions, including extraction/nanoESI solvent composition, volume, and dwell times, were optimized in the analysis of targeted compounds. Limit of detection and quantitation as well as analysis reproducibility figures of merit were measured. Calibration data was obtained for propranolol using a deuterated internal standard which demonstrated linearity and reproducibility. A 10x increase in signal and cleanup of micromolar Angiotensin II from a concentrated salt solution was demonstrated. Additionally, a multicomponent herbicide mixture at ppb concentration levels was analyzed using MS3 spectra for compound identification in the presence of isobaric interferences.

  11. Quantitative analysis of paraquat in vegetation by stable isotope dilution and liquid chromatography/electrospray ionization-mass spectrometry. (United States)

    Schaner, Angela; Hickes, Heidi


    The method presented is a suitable approach for routine testing of paraquat in difficult sample types, such as winter wheat and alfalfa plant tissue, typically found with accidental spray drift. Hydrophilic interaction chromatography and ultra-performance LC is utilized with tandem quadrupole MS in the positive electrospray ionization mode. Three precursor-product ion transitions are measured in the multiple reaction monitoring mode, and paraquat d8 is added as an internal standard at the beginning of the extraction procedure to correct for losses in recovery and/or matrix effects in instrument response. A 5 g portion is digested with 6 M HCl in a 100°C water bath for 1 h. An aliquot is removed and adjusted to pH 7-8 prior to loading on a mixed mode weak cation-exchange SPE cartridge, and paraquat is eluted with formic acid-acetonitrile (10 + 90, v/v). Average recoveries of paraquat fortified at 0.020-0.080 ppm in winter wheat and alfalfa ranged from 80 to 114% (RSD 12-30%). Result data from naturally incurred paraquat (0.027-0.51 ppm) in composite garden plants, potato leaves, tree leaves, and alfalfa are presented. The LOQ is 0.020 ppm.

  12. Analysis preliminary phytochemical raw extract of leaves Nephrolepis pectinata

    Directory of Open Access Journals (Sweden)

    Natally Marreiros Gomes


    Full Text Available The Nephrolepis pectinata popularly known as paulista fern, ladder-heaven, cat tail, belongs to the family Davalliaceae. For the beauty of the arrangements of their leaves ferns are quite commercialized in Brazil, however, have not been described in the literature studies on their pharmacological potential. Thus, the objective of this research was to analyze the phytochemical properties of the crude extract of the leaves of Nephrolepis pectinata. To perform the phytochemical analysis were initially made the collection of the vegetable, preparation of voucher specimen, washing, drying and grinding. Then, extraction by percolation method and end the phytochemical analysis. Preliminary results phytochemicals the crude extract of the leaves of Nephrolepis pectinata tested positive for reducing sugars, phenols/tannins (catechins tannins and catechins.

  13. Single corn kernel aflatoxin B1 extraction and analysis method (United States)

    Aflatoxins are highly carcinogenic compounds produced by the fungus Aspergillus flavus. Aspergillus flavus is a phytopathogenic fungus that commonly infects crops such as cotton, peanuts, and maize. The goal was to design an effective sample preparation method and analysis for the extraction of afla...

  14. Preprocessing and exploratory analysis of chromatographic profiles of plant extracts

    NARCIS (Netherlands)

    Hendriks, M.M.W.B.; Cruz-Juarez, L.; Bont, de D.; Hall, R.D.


    The characterization of herbal extracts to compare samples from different origin is important for robust production and quality control strategies. This characterization is now mainly performed by analysis of selected marker compounds. Metabolic fingerprinting of full metabolite profiles of plant ex

  15. Chemical analysis of Ginkgo biloba leaves and extracts

    NARCIS (Netherlands)

    Beek, van T.A.


    The chemical analysis and quality control of Ginkgo leaves and extracts is reviewed. Important constituents present in the medicinally used leaves are the terpene trilactones, i.e., ginkgolides A, B, C, J and bilobalide, many flavonol glycosides, biflavones, proanthocyanidins, alkylphenols, simple p

  16. Thin-layer chromatography/direct analysis in real time time-of-flight mass spectrometry and isotope dilution to analyze organophosphorus insecticides in fatty foods. (United States)

    Kiguchi, Osamu; Oka, Kazuko; Tamada, Masafumi; Kobayashi, Takashi; Onodera, Jun


    To assess food safety emergencies caused by highly hazardous chemical-tainted foods, simultaneous analysis of organophosphorus insecticides in fatty foods such as precooked foods was conducted using thin-layer chromatography/direct analysis in real time time-of-flight mass spectrometry (TLC/DART-TOFMS) and isotope dilution technique. Polar (methamidophos and acephate) and nonpolar organophosphorus insecticides (fenitrothion, diazinon, and EPN) were studied. Experiments to ascertain chromatographic patterns using TLC/DART-TOFMS reveal that it was more useful than GC/MS or GC/MS/MS for the simultaneous analyses of polar and nonpolar pesticides, while obviating the addition of a protective agent for tailing effects of polar pesticides. Lower helium gas temperature (260°C) for DART-TOFMS was suitable for the simultaneous analysis of target pesticides. Linearities were achieved respectively at a lower standard concentration range (0.05-5 μg) for diazinon and EPN and at a higher standard concentration range (2.5-25 μg) for methamidophos, acephate, and fenitrothion. Their respective coefficients of determination were ≥ 0.9989 and ≥ 0.9959. A few higher repeatabilities (RSDs) for diazinon and EPN were found (>20%), although isotope dilution technique was used. Application to the HPTLC plate without an automatic TLC sampler might be inferred as a cause of their higher RSDs. Detection limits were estimated in the higher picogram range for diazinon and EPN, and in the lower nanogram range for methamidophos, acephate, and fenitrothion. Aside from methamidophos, recovery results (n=3) obtained using a highly insecticide-tainted fatty food (dumpling) and raw food (grapefruit) samples (10mg/kg) using TLC/DART-TOFMS with both complex and simpler cleanups were not as susceptible to matrix effects (95-121%; RSD, 1.3-14%) as those using GC/MS/MS (102-117%; RSD, 0.4-8.5%), although dumpling samples using GC/MS were remarkably susceptible to matrix effects. The coupled method of

  17. Phytochemicals analysis and medicinal potentials of hydroalcoholic extract from Curtisia dentata (Burm.f) C.A. Sm Stem Bark. (United States)

    Oyedemi, Sunday Oyewole; Oyedemi, Blessing Ogochukwuamaka; Arowosegbe, Sunday; Afolayan, Anthony Jide


    Curtisia dentata (CD) is a vulnerable medicinal plant used for the treatment of stomach ailments in South Africa. However, there is a lack of sufficient data on its phytochemical components and medicinal properties. The phytochemical analysis of the extract was estimated using standard assay methods while its antibacterial activity was determined by the agar dilution method against selected bacteria. The antioxidant activity of the extract was done using ferric reducing power, 1,1-diphenyl-2-picrylhydrazyl (DPPH), 2,2'-azino-bis-3-ethylbenzothiazoline-6-sulfonic-acid (ABTS), nitric oxide (NO), hydrogen peroxide (H(2)O(2)) and lipid peroxidation (LPO). The cytotoxicity assay of the extract was assessed using the brine shrimp lethality test with LC(50) value of 0.302 mg/mL. The antibacterial activity of the extract demonstrated an appreciable broad spectrum activity against the tested bacteria with minimum inhibitory concentration (MIC) ranges between 5000 and 0.5 mg/L. Both phenol and flavonoid concentrations were 14.86 mg tannic acid equivalent/g and 13.64 mg quercetin equivalent/g, respectively. The percentage composition of saponins (13.26) was highest, followed by steroids (1.42), while alkaloids and tannins had the same value of 0.51. Similarly, IC(50) values of the extract against DPPH, ABTS, H(2)O(2), LPO and NO were 0.017, 0.018, 0.159, 0.06 and 0.052 mg/mL, respectively. The reducing power of the extract was found to be concentration dependent. Our data suggest that the 70% ethanol extract from the CD extract has antibacterial and antioxidant properties due to the presence of bio-active compounds and thus support its folkloric use in the treatment of diseases.

  18. Rapid automatic keyword extraction for information retrieval and analysis (United States)

    Rose, Stuart J [Richland, WA; Cowley,; E, Wendy [Richland, WA; Crow, Vernon L [Richland, WA; Cramer, Nicholas O [Richland, WA


    Methods and systems for rapid automatic keyword extraction for information retrieval and analysis. Embodiments can include parsing words in an individual document by delimiters, stop words, or both in order to identify candidate keywords. Word scores for each word within the candidate keywords are then calculated based on a function of co-occurrence degree, co-occurrence frequency, or both. Based on a function of the word scores for words within the candidate keyword, a keyword score is calculated for each of the candidate keywords. A portion of the candidate keywords are then extracted as keywords based, at least in part, on the candidate keywords having the highest keyword scores.

  19. Design and Implementation of SMS Extraction and Analysis System

    Directory of Open Access Journals (Sweden)

    Wan Yu-Yang


    Full Text Available With more and more applications of smart phone, more and more text messages in mobile phone, and then more and more information possibly contained in text messages. How to dig out useful information form SMS? This paper discusses techniques of the SMS extraction and analysis. Taking the bank SMS as example, key information is extracted to inform, is formatted to story in APP database, and then be analysed and statistic result shown in chart. The APP with the function is run well on Android phone and has Practical value. This technology helps to expand the application of SMS.

  20. Features extraction in anterior and posterior cruciate ligaments analysis. (United States)

    Zarychta, P


    The main aim of this research is finding the feature vectors of the anterior and posterior cruciate ligaments (ACL and PCL). These feature vectors have to clearly define the ligaments structure and make it easier to diagnose them. Extraction of feature vectors is obtained by analysis of both anterior and posterior cruciate ligaments. This procedure is performed after the extraction process of both ligaments. In the first stage in order to reduce the area of analysis a region of interest including cruciate ligaments (CL) is outlined in order to reduce the area of analysis. In this case, the fuzzy C-means algorithm with median modification helping to reduce blurred edges has been implemented. After finding the region of interest (ROI), the fuzzy connectedness procedure is performed. This procedure permits to extract the anterior and posterior cruciate ligament structures. In the last stage, on the basis of the extracted anterior and posterior cruciate ligament structures, 3-dimensional models of the anterior and posterior cruciate ligament are built and the feature vectors created. This methodology has been implemented in MATLAB and tested on clinical T1-weighted magnetic resonance imaging (MRI) slices of the knee joint. The 3D display is based on the Visualization Toolkit (VTK).

  1. Cloud point extraction for analysis of antiretrovirals in human plasma by UFLC-ESI-MS/MS

    Directory of Open Access Journals (Sweden)

    Gabriel A. Hunzicker


    Full Text Available An analytical methodology based on cloud point extraction (CPE coupled to Ultra-Fast Liquid Chromatography and electrospray tandem mass spectrometry (UFLC-MS/MS was developed for analysis of Abacavir (ABC, Efavirenz (EFV, Lamivudine (3 TC and Nelfinavir (NFV in human plasma. It is the first time that CPE was used for extraction of antiretrovirals (ARV from plasma. The effects of relevant physic-chemical variables on analytical response of each ARV, including pH, surfactant concentration, equilibration time and temperature, were study and optimized; as well as its coupling to UFLC-ESI-MS/MS. Under optimized conditions, the resulting methodology was as follows: a 500 μL aliquot of human plasma was diluted with 2 mL deionized water in a 10 mL centrifuge tube. A 500 μL aliquot Triton X-114 5% w/v was added and homogenized using a vortex stirrer. The resulting cloudy solution was kept at 65 °C for 20 min for promoting the condensation of surfactant micelles. Then it was centrifuged at 3000 × g for 5 min for separation of the surfactant-rich phase. After discarding the aqueous supernatant, 400 μL ACN were added to the remaining surfactant rich phase and centrifuged in order to precipitate proteins and separate them. A 150 μL aliquot of the supernatant was transferred to 2 mL vial and further diluted with 400 μL deionized water. A 30 μL aliquot of the so-prepared solution was injected and analyzed into the UFLC-MS/MS. The method detection limits for ABC, EFV, 3 TC and NFV under optimized conditions were 31, 77, 57 and 21 ng mL−1, respectively. The RSD% for the studied analytes were <15%, except at the LOQ, which were <19%. Recovery values ranged from 81 to 107%. The proposed methodology was successfully applied for the analysis of ABC, EFV, 3 TC and NFV in human plasma within the concentration range of 43–6816, 125–4992, 81–3248 and 49–7904 ng mL−1, respectively. Under optimized working conditions the proposed

  2. Evolution of Analysis of Polyhenols from Grapes, Wines, and Extracts

    Directory of Open Access Journals (Sweden)

    Pierre-Louis Teissedre


    Full Text Available Grape and wine phenolics are structurally diverse, from simple molecules to oligomers and polymers usually designated as tannins. They have an important impact on the organoleptic properties of wines, that’s why their analysis and quantification are of primordial importance. The extraction of phenolics from grapes and from wines is the first step involved in the analysis. Then, several analytical methods have been developed for the determination of total content of phenolic, while chromatographic and spectrophotometric analyses are continuously improved in order to achieve adequate separation of phenolic molecules, their subsequent identification and quantification. This review provides a summary of evolution of analysis of polyphenols from grapes, wines and extracts.

  3. Social network extraction and analysis based on multimodal dyadic interaction. (United States)

    Escalera, Sergio; Baró, Xavier; Vitrià, Jordi; Radeva, Petia; Raducanu, Bogdan


    Social interactions are a very important component in people's lives. Social network analysis has become a common technique used to model and quantify the properties of social interactions. In this paper, we propose an integrated framework to explore the characteristics of a social network extracted from multimodal dyadic interactions. For our study, we used a set of videos belonging to New York Times' Blogging Heads opinion blog. The Social Network is represented as an oriented graph, whose directed links are determined by the Influence Model. The links' weights are a measure of the "influence" a person has over the other. The states of the Influence Model encode automatically extracted audio/visual features from our videos using state-of-the art algorithms. Our results are reported in terms of accuracy of audio/visual data fusion for speaker segmentation and centrality measures used to characterize the extracted social network.

  4. Social Network Extraction and Analysis Based on Multimodal Dyadic Interaction

    Directory of Open Access Journals (Sweden)

    Bogdan Raducanu


    Full Text Available Social interactions are a very important component in people’s lives. Social network analysis has become a common technique used to model and quantify the properties of social interactions. In this paper, we propose an integrated framework to explore the characteristics of a social network extracted from multimodal dyadic interactions. For our study, we used a set of videos belonging to New York Times’ Blogging Heads opinion blog. The Social Network is represented as an oriented graph, whose directed links are determined by the Influence Model. The links’ weights are a measure of the “influence” a person has over the other. The states of the Influence Model encode automatically extracted audio/visual features from our videos using state-of-the art algorithms. Our results are reported in terms of accuracy of audio/visual data fusion for speaker segmentation and centrality measures used to characterize the extracted social network.

  5. Microscale extraction method for HPLC carotenoid analysis in vegetable matrices

    Directory of Open Access Journals (Sweden)

    Sidney Pacheco


    Full Text Available In order to generate simple, efficient analytical methods that are also fast, clean, and economical, and are capable of producing reliable results for a large number of samples, a micro scale extraction method for analysis of carotenoids in vegetable matrices was developed. The efficiency of this adapted method was checked by comparing the results obtained from vegetable matrices, based on extraction equivalence, time required and reagents. Six matrices were used: tomato (Solanum lycopersicum L., carrot (Daucus carota L., sweet potato with orange pulp (Ipomoea batatas (L. Lam., pumpkin (Cucurbita moschata Duch., watermelon (Citrullus lanatus (Thunb. Matsum. & Nakai and sweet potato (Ipomoea batatas (L. Lam. flour. Quantification of the total carotenoids was made by spectrophotometry. Quantification and determination of carotenoid profiles were formulated by High Performance Liquid Chromatography with photodiode array detection. Microscale extraction was faster, cheaper and cleaner than the commonly used one, and advantageous for analytical laboratories.

  6. Molecularly Imprinted Polymers for Ochratoxin A Extraction and Analysis

    Directory of Open Access Journals (Sweden)

    Jorn C. C. Yu


    Full Text Available Molecularly imprinted polymers (MIPs are considered as polymeric materials that mimic the functionality of antibodies. MIPs have been utilized for a wide variety of applications in chromatography, solid phase extraction, immunoassays, and sensor recognition. In this article, recent advances of MIPs for the extraction and analysis of ochratoxins are discussed. Selection of functional monomers to bind ochratoxin A (OTA with high affinities, optimization of extraction procedures, and limitations of MIPs are compared from different reports. The most relevant examples in the literature are described to clearly show how useful these materials are. Strategies on MIP preparation and schemes of analytical methods are also reviewed in order to suggest the next step that would make better use of MIPs in the field of ochratoxin research. The review ends by outlining the remaining issues and impediments.

  7. Surface-activated chemical ionization ion trap mass spectrometry in the analysis of amphetamines in diluted urine samples. (United States)

    Cristoni, Simone; Bernardi, Luigi Rossi; Gerthoux, Piermario; Gonella, Elisabetta; Mocarelli, Paolo


    A new ionization method, named surface-activated chemical ionization (SACI), was employed for the analysis of five amphetamines (3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyethylamphetamine (MDE), amphetamine and methamphetamine) by ion trap mass spectrometry. The results so obtained have been compared with those achieved by using atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) using the same instrument, clearly showing that SACI is the most sensitive of the three. The limit of detection and linearity range for SACI were compared with those obtained using APCI and ESI, showing that the new SACI approach provides the best results for both criteria. SACI was used to analyze MDA, MDMA MDE, amphetamine and methamphetamine in four urine samples, and the quantitation results are compared with those achieved using ESI.

  8. Global transcriptome analysis of Clostridium thermocellum ATCC 27405 during growth on dilute acid pretreated Populus and switchgrass

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, Charlotte M [ORNL; Rodriguez Jr, Miguel [ORNL; Johnson, Courtney M [ORNL; Martin, S L. [North Carolina State University; Chu, Tzu Ming [SAS Institute; Wolfinger, Russ [SAS Institute; Hauser, Loren John [ORNL; Land, Miriam L [ORNL; Klingeman, Dawn Marie [ORNL; Tschaplinski, Timothy J [ORNL; Mielenz, Jonathan R [ORNL; Brown, Steven D [ORNL


    Background The thermophilic anaerobe Clostridium thermocellum is a candidate consolidated bioprocessing (CBP) biocatalyst for cellulosic ethanol production. The aim of this study was to investigate C. thermocellum genes required to ferment biomass substrates and to conduct a robust comparison of DNA microarray and RNA sequencing (RNA-seq) analytical platforms. Results C. thermocellum ATCC 27405 fermentations were conducted with a 5 g/L solid substrate loading of either pretreated switchgrass or Populus. Quantitative saccharification and inductively coupled plasma emission spectroscopy (ICP-ES) for elemental analysis revealed composition differences between biomass substrates, which may have influenced growth and transcriptomic profiles. High quality RNA was prepared for C. thermocellum grown on solid substrates and transcriptome profiles were obtained for two time points during active growth (12 hours and 37 hours postinoculation). A comparison of two transcriptomic analytical techniques, microarray and RNA-seq, was performed and the data analyzed for statistical significance. Large expression differences for cellulosomal genes were not observed. We updated gene predictions for the strain and a small novel gene, Cthe_3383, with a putative AgrD peptide quorum sensing function was among the most highly expressed genes. RNAseq data also supported different small regulatory RNA predictions over others. The DNA microarray gave a greater number (2,351) of significant genes relative to RNA-seq (280 genes when normalized by the kernel density mean of M component (KDMM) method) in an analysis of variance (ANOVA) testing method with a 5 % false discovery rate (FDR). When a 2-fold difference in expression threshold was applied, 73 genes were significantly differentially expressed in common between the two techniques. Sulfate and phosphate uptake/utilization genes, along with genes for a putative efflux pump system were some of the most differentially regulated transcripts

  9. Internal correction of hafnium oxide spectral interferences and mass bias in the determination of platinum in environmental samples using isotope dilution analysis. (United States)

    Rodríguez-Castrillón, José Angel; Moldovan, Mariella; García Alonso, J Ignacio


    A method has been developed for the accurate determination of platinum by isotope dilution analysis, using enriched (194)Pt, in environmental samples containing comparatively high levels of hafnium without any chemical separation. The method is based on the computation of the contribution of hafnium oxide as an independent factor in the observed isotope pattern of platinum in the spiked sample. Under these conditions, the ratio of molar fractions between natural abundance and isotopically enriched platinum was independent of the amount of hafnium present in the sample. Additionally, mass bias was corrected by an internal procedure in which the regression variance was minimised. This was possible as the mass bias factor for hafnium oxide was very close to that of platinum. The final procedure required the measurement of three platinum isotope ratios (192/194, 195/194 and 196/194) to calculate the concentration of platinum in the sample. The methodology has been validated using the reference material "BCR-723 road dust" and has been applied to different environmental matrices (road dust, air particles, bulk wet deposition and epiphytic lichens) collected in the Aspe Valley (Pyrenees Mountains). A full uncertainty budget, using Kragten's spreadsheet method, showed that the total uncertainty was limited only by the uncertainty in the measured isotope ratios and not by the uncertainties of the isotopic composition of platinum and hafnium.

  10. Development of a routine analysis of 4-mercapto-4-methylpentan-2-one in wine by stable isotope dilution assay and mass tandem spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Dagan, Laurent; Reillon, Florence; Roland, Aurélie; Schneider, Rémi, E-mail:


    Highlights: • We proposed a routine method to analyze the 4-methyl-4-mercaptopentan-2-one in wine. • We developed the first method with sensitivity below the 4MMP perception threshold. • We obtained an accurate method by using the stable isotope dilution assay approach. Abstract: The 4-mercapto-4-methylpentan-2-one (4MMP) is a key aroma compound in wines, especially in Sauvignon Blanc ones. Its accurate quantification is quite difficult due to its traces levels and its reactivity in wine conferred by the thiol function. In this paper, we proposed a new method for its quantification in wine without any sample preparation, based on automated derivatization procedure by methoximation and SIDA–SPME–GC–MS/MS analysis. The derivatization procedure was adapted from a previously published method in order to decrease the amount of reagents and the volume of wine (only 3 mL are required). The use of SPME and the detection conditions have also been optimized to reach the best sensitivity as possible. The method was then validated according to the International Organization of Vine and Wine recommendations and exhibited excellent performances. Indeed, this method allowed us to quantify the 4MMP in wine at traces levels (LOD = 0.19 ng L₅⁻¹) with reproducible results (RSD < 15%) and a very good accuracy (recovery = 102%)

  11. Mass spectrometric profiling of Bacillus cereus strains and quantitation of the emetic toxin cereulide by means of stable isotope dilution analysis and HEp-2 bioassay. (United States)

    Stark, Timo; Marxen, Sandra; Rütschle, Andrea; Lücking, Genia; Scherer, Siegfried; Ehling-Schulz, Monika; Hofmann, Thomas


    A fast and robust high-throughput ultra-performance liquid chromatography/time-of-flight mass spectrometry (UPLC-TOF MS) profiling method was developed and successfully applied to discriminate a total of 78 Bacillus cereus strains into no/low, medium and high producers of the emetic toxin cereulide. The data obtained by UPLC-TOF MS profiling were confirmed by absolute quantitation of cereulide in selected samples by means of high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS) and stable isotope dilution assay (SIDA). Interestingly, the B. cereus strains isolated from four vomit samples and five faeces samples from patients showing symptoms of intoxication were among the group of medium or high producers. Comparison of HEp-2 bioassay data with those determined by means of mass spectrometry showed differences, most likely because the HEp-2 bioassay is based on the toxic action of cereulide towards mitochondria of eukaryotic cells rather than on a direct measurement of the toxin. In conclusion, the UPLC-electrospray ionization (ESI)-TOF MS and the HPLC-ESI-MS/MS-SIDA analyses seem to be promising tools for the robust high-throughput analysis of cereulide in B. cereus cultures, foods and other biological samples.


    Afzal, Samina; Chaudhary, Bashir Ahmad; Ahmad, Ashfaq; Afzali, Khurram


    Zaleya pentandra (Zp) and Cochoms depressus Linn. (Cd) have been considered as herbs with potential therapeutic benefits. Zp and Cd belong to the important family Aizoaceae and Tiliaceae, respectively. The extractions were carried out successively with methanol and dichloromethane at room temperature for 24 h. Preliminary phytochemical screening of Zp and Cd revealed the presence of steroids, alkaloids, saponins, and anthraquinones. The methanolic and dichloromethane extracts of selected plants were subjected to examination of antifungal activity by using agar tube dilution. The extracts were tested against different fungi such as A. nigeir, A. flavus, F. solani, A. funigatis and Mucor. The dichloromethane extract of aerial parts of Cd showed high antifungal activity against A. niger as compared to all other tested extracts.

  13. Improved ethanol yield and reduced minimum ethanol selling price (MESP by modifying low severity dilute acid pretreatment with deacetylation and mechanical refining: 2 Techno-economic analysis

    Directory of Open Access Journals (Sweden)

    Tao Ling


    Full Text Available Abstract Background Our companion paper discussed the yield benefits achieved by integrating deacetylation, mechanical refining, and washing with low acid and low temperature pretreatment. To evaluate the impact of the modified process on the economic feasibility, a techno-economic analysis (TEA was performed based on the experimental data presented in the companion paper. Results The cost benefits of dilute acid pretreatment technology combined with the process alternatives of deacetylation, mechanical refining, and pretreated solids washing were evaluated using cost benefit analysis within a conceptual modeling framework. Control cases were pretreated at much lower acid loadings and temperatures than used those in the NREL 2011 design case, resulting in much lower annual ethanol production. Therefore, the minimum ethanol selling prices (MESP of the control cases were $0.41-$0.77 higher than the $2.15/gallon MESP of the design case. This increment is highly dependent on the carbohydrate content in the corn stover. However, if pretreatment was employed with either deacetylation or mechanical refining, the MESPs were reduced by $0.23-$0.30/gallon. Combing both steps could lower the MESP further by $0.44 ~ $0.54. Washing of the pretreated solids could also greatly improve the final ethanol yields. However, the large capital cost of the solid–liquid separation unit negatively influences the process economics. Finally, sensitivity analysis was performed to study the effect of the cost of the pretreatment reactor and the energy input for mechanical refining. A 50% cost reduction in the pretreatment reactor cost reduced the MESP of the entire conversion process by $0.11-$0.14/gallon, while a 10-fold increase in energy input for mechanical refining will increase the MESP by $0.07/gallon. Conclusion Deacetylation and mechanical refining process options combined with low acid, low severity pretreatments show improvements in ethanol yields and

  14. Ground extraction from airborne laser data based on wavelet analysis (United States)

    Xu, Liang; Yang, Yan; Jiang, Bowen; Li, Jia


    With the advantages of high resolution and accuracy, airborne laser scanning data are widely used in topographic mapping. In order to generate a DTM, measurements from object features such as buildings, vehicles and vegetation have to be classified and removed. However, the automatic extraction of bare earth from point clouds acquired by airborne laser scanning equipment remains a problem in LIDAR data filtering nowadays. In this paper, a filter algorithm based on wavelet analysis is proposed. Relying on the capability of detecting discontinuities of continuous wavelet transform and the feature of multi-resolution analysis, the object points can be removed, while ground data are preserved. In order to evaluate the performance of this approach, we applied it to the data set used in the ISPRS filter test in 2003. 15 samples have been tested by the proposed approach. Results showed that it filtered most of the objects like vegetation and buildings, and extracted a well defined ground model.

  15. Blind Extraction and Security Analysis of Spread Spectrum Hidden Watermarks (United States)


    DATES COVERED (From - To) JAN 2009 – DEC 2010 4. TITLE AND SUBTITLE BLIND EXTRACTION AND SECURITY ANALYSIS OF SPREAD SPECTRUM HIDDEN WATERMARKS ...Multi Signature Embedding, Watermarking , DSSS. 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT UU 18. NUMBER OF PAGES 15 19a... watermarks John A. Marsh*a,b, and Gerard F. Wohlrabc aSUNY Institute of Technology, 100 Seymour Dr., Utica, NY 13502; bAssured Information

  16. User Suggestions Extraction from customer Reviews A Sentiment Analysis approach

    Directory of Open Access Journals (Sweden)



    Full Text Available Customer review is a major criterion for the improvement of the quality of services rendered and enhancement of the deliverables. Blogs, articles and discussion forums, provide manufacturers or sellers with a good understanding of the reception level of their products in the competitive market. An interesting area from the business analysis perspective, this paper discusses an opinion based mining technique for the extraction of the relevant data using Natural Language Processing and text analysis, and comprehends suggestions from an actionable feedback.

  17. Isotope dilution analysis of polychlorinated biphenyls (PCBs) in transformer oil and global commercial PCB formulations by high resolution gas chromatography-high resolution mass spectrometry. (United States)

    Takasuga, Takumi; Senthilkumar, Kurunthachalam; Matsumura, Tohru; Shiozaki, Ken; Sakai, Shin-ichi


    Special polychlorinated biphenyls (PCBs) standards (native and isotope labeled) were analyzed by isotope dilution method using HRGC-HRMS. Multiple analysis of special PCBs standards by three different laboratories produced the relative response factors (RRFs) and relative standard deviations (RSDs %) was in the average of 0.979 and 3.86, respectively. Additionally, inter-laboratory analysis of various forms of transformer oil revealed the PCBs concentrations were in the following order; PCBs fortified transformer oil (940-1300 ng/g)>PCB polluted transformer oil (490-680 ng/g)>chemically degraded-transformer oil (480-490 ng/g) and PCBs free oil (ND-17 ng/g). Chemical degradation resulted in an order of magnitude decrease in the PCB concentrations. Specifically, higher chlorinated PCBs degraded into lower chlorinated PCBs. Also, composition of PCBs have been determined in PCB formulations from Japan (Kanechlor), Germany (Clophen), USA (Aroclor), Russia (Sovol) and Poland (Chlorofen). Major PCBs (24-PCB congeners) contributed 54-67%, 55-68%, 16-69%, 71% and 72% in Kanechlor, Clophen, Aroclor, Sovol and Chlorofen, respectively to total PCBs. The homologue pattern of Kanechlor, Aroclor and Clophen in technical fromulation was similar (e.g., Kanechlor-300 resembled to those of Clophen A-30 and Aroclor-1242). Furthermore, congener-specific distributions of major PCBs/dioxin-like PCBs and toxic equivalency quantities (TEQ) were calculated. Based on our tentative assumption calculations, cumulative production of five different technical PCB formulations, WHO-TEQ emission was estimated to be approximately 16.05 tons.


    DEFF Research Database (Denmark)

    Pafilis, Evangelos; Buttigieg, Pier Luigi; Ferrell, Barbra


    The microbial and molecular ecology research communities have made substantial progress on developing standards for annotating samples with environment metadata. However, sample manual annotation is a highly labor intensive process and requires familiarity with the terminologies used. We have the...... and text-mining-assisted curation revealed that EXTRACT speeds up annotation by 15-25% and helps curators to detect terms that would otherwise have been missed.Database URL:

  19. Over-evaluation of total flavonoids in grape skin extracts containing sulphur dioxide. (United States)

    Corona, Onofrio; Squadrito, Margherita; Vento, Giorgia; Tirelli, Antonio; Di Stefano, Rocco


    Sulphur dioxide (SO2) proved to increase absorbance at 280 nm of grape skin and seed extracts containing it, diluted with ethanol-HCl to assess total flavonoids and anthocyanins in the same analysis. Additional absorbance at 280 nm was also observed in acetone:H2O extracts, if the acetone had not completely evaporated before the extracts were diluted with a solvent. Flavonoids were correctly quantified in the extracts when SO2 or acetone were removed by solid-phase extraction with a C18 RP as sorbent and methanol as eluting solvent.

  20. Microwave-assisted extraction versus Soxhlet extraction for the analysis of short-chain chlorinated alkanes in sediments. (United States)

    Parera, J; Santos, F J; Galceran, M T


    Microwave-assisted extraction (MAE) was evaluated as a possible alternative to Soxhlet extraction for analysing short-chain chlorinated alkanes (commonly called short-chain chlorinated paraffins, SCCPs) in river sediment samples, using gas chromatography coupled to negative chemical ionisation mass spectrometry. For MAE optimisation, several extraction parameters such as solvent extraction mixture, extraction time and extraction temperature were studied. Maximum extraction efficiencies for SCCPs (90%) and for 12 polychlorinated biphenyl (PCB) congeners (91-95%) were achieved using 5 g of sediment sample, 30 ml of n-hexane-acetone (1:1, v/v) as solvent extraction, and 15 min and 115 degrees C of extraction time and temperature, respectively. Activated Florisil was used to clean-up the extracts, allowing highly selective separation of SCCPs from other organic contaminants such as PCBs. MAE was compared with a conventional extraction technique such as Soxhlet and good agreement in the results was obtained. Quality parameters of the optimised MAE method such as run-to-run (R.S.D. 7%) and day-to-day precision (R.S.D. 9%) were determined using spiked river sediment samples, with LODs of 1.5 ng g(-1). This method was successfully applied to the analysis of SCCPs in river sediment samples at concentrations below the ng g(-1) level. O 2004 Elsevier B.V. All rights reserved.

  1. Plant Phenolics: Extraction, Analysis and Their Antioxidant and Anticancer Properties

    Directory of Open Access Journals (Sweden)

    Jin Dai


    Full Text Available Phenolics are broadly distributed in the plant kingdom and are the most abundant secondary metabolites of plants. Plant polyphenols have drawn increasing attention due to their potent antioxidant properties and their marked effects in the prevention of various oxidative stress associated diseases such as cancer. In the last few years, the identification and development of phenolic compounds or extracts from different plants has become a major area of health- and medical-related research. This review provides an updated and comprehensive overview on phenolic extraction, purification, analysis and quantification as well as their antioxidant properties. Furthermore, the anticancer effects of phenolics in-vitro and in-vivo animal models are viewed, including recent human intervention studies. Finally, possible mechanisms of action involving antioxidant and pro-oxidant activity as well as interference with cellular functions are discussed.

  2. Optimized protein extraction methods for proteomic analysis of Rhizoctonia solani. (United States)

    Lakshman, Dilip K; Natarajan, Savithiry S; Lakshman, Sukla; Garrett, Wesley M; Dhar, Arun K


    Rhizoctonia solani (Teleomorph: Thanatephorus cucumeris, T. praticola) is a basidiomycetous fungus and a major cause of root diseases of economically important plants. Various isolates of this fungus are also beneficially associated with orchids, may serve as biocontrol agents or remain as saprophytes with roles in decaying and recycling of soil organic matter. R. solani displays several hyphal anastomosis groups (AG) with distinct host and pathogenic specializations. Even though there are reports on the physiological and histological basis of Rhizoctonia-host interactions, very little is known about the molecular biology and control of gene expression early during infection by this pathogen. Proteamic technologies are powerful tools for examining alterations in protein profiles. To aid studies on its biology and host pathogen interactions, a two-dimensional (2-D) gel-based global proteomic study has been initiated. To develop an optimized protein extraction protocol for R. solani, we compared two previously reported protein extraction protocols for 2-D gel analysis of R. solani (AG-4) isolate Rs23. Both TCA-acetone precipitation and phosphate solubilization before TCA-acetone precipitation worked well for R. solani protein extraction, although selective enrichment of some proteins was noted with either method. About 450 spots could be detected with the densitiometric tracing of Coomassie blue-stained 2-D PAGE gels covering pH 4-7 and 6.5-205 kDa. Selected protein spots were subjected to mass spectrometric analysis with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS). Eleven protein spots were positively identified based on peptide mass fingerprinting match with fungal proteins in public databases with the Mascot search engine. These results testify to the suitability of the two optimized protein extraction protocols for 2-D proteomic studies of R. solani.

  3. Extraction and Quantitative HPLC Analysis of Coumarin in Hydroalcoholic Extracts of Mikania glomerata Spreng: ("guaco" Leaves

    Directory of Open Access Journals (Sweden)

    Celeghini Renata M. S.


    Full Text Available Methods for preparation of hydroalcoholic extracts of "guaco" (Mikania glomerata Spreng. leaves were compared: maceration, maceration under sonication, infusion and supercritical fluid extraction. Evaluation of these methods showed that maceration under sonication had the best results, when considering the ratio extraction yield/extraction time. A high performance liquid chromatography (HPLC procedure for the determination of coumarin in these hydroalcoholic extracts of "guaco" leaves is described. The HPLC method is shown to be sensitive and reproducible.

  4. Entropy Analysis as an Electroencephalogram Feature Extraction Method

    Directory of Open Access Journals (Sweden)

    P. I. Sotnikov


    Full Text Available The aim of this study was to evaluate a possibility for using an entropy analysis as an electroencephalogram (EEG feature extraction method in brain-computer interfaces (BCI. The first section of the article describes the proposed algorithm based on the characteristic features calculation using the Shannon entropy analysis. The second section discusses issues of the classifier development for the EEG records. We use a support vector machine (SVM as a classifier. The third section describes the test data. Further, we estimate an efficiency of the considered feature extraction method to compare it with a number of other methods. These methods include: evaluation of signal variance; estimation of spectral power density (PSD; estimation of autoregression model parameters; signal analysis using the continuous wavelet transform; construction of common spatial pattern (CSP filter. As a measure of efficiency we use the probability value of correctly recognized types of imagery movements. At the last stage we evaluate the impact of EEG signal preprocessing methods on the final classification accuracy. Finally, it concludes that the entropy analysis has good prospects in BCI applications.

  5. Luminescence properties of dilute bismide systems

    Energy Technology Data Exchange (ETDEWEB)

    Breddermann, B., E-mail: [Faculty of Physics, Philipps-Universität Marburg, 35032 Marburg (Germany); Bäumner, A.; Koch, S.W.; Ludewig, P.; Stolz, W.; Volz, K. [Faculty of Physics, Philipps-Universität Marburg, 35032 Marburg (Germany); Hader, J.; Moloney, J.V. [Nonlinear Control Strategies Inc, 3542 N. Geronimo Ave., Tucson, AZ 85705 (United States); Broderick, C.A.; O' Reilly, E.P. [Tyndall National Institute, Lee Maltings, Dyke Parade, Cork (Ireland); Department of Physics, University College Cork, Cork (Ireland)


    Systematic photoluminescence measurements on a series of GaBi{sub x}As{sub 1−x} samples are analyzed theoretically using a fully microscopic approach. Based on sp{sup 3}s{sup ⁎} tight-binding calculations, an effective k·p model is set up and used to compute the band structure and dipole matrix elements for the experimentally investigated samples. With this input, the photoluminescence spectra are calculated using a systematic microscopic approach based on the semiconductor luminescence equations. The detailed theory-experiment comparison allows us to quantitatively characterize the experimental structures and to extract important sample parameters. - Highlights: • Measurement of photoluminescence spectra of a home grown series of dilute bismides. • Fully microscopic calculation of luminescence spectra from detailed band structure. • Quantitative experiment-theory comparison of luminescence spectra. • Thorough understanding of optoelectronic properties of dilute bismide material system. • Promising perspectives for the development of new device applications.

  6. Independent component analysis for automatic note extraction from musical trills (United States)

    Brown, Judith C.; Smaragdis, Paris


    The method of principal component analysis, which is based on second-order statistics (or linear independence), has long been used for redundancy reduction of audio data. The more recent technique of independent component analysis, enforcing much stricter statistical criteria based on higher-order statistical independence, is introduced and shown to be far superior in separating independent musical sources. This theory has been applied to piano trills and a database of trill rates was assembled from experiments with a computer-driven piano, recordings of a professional pianist, and commercially available compact disks. The method of independent component analysis has thus been shown to be an outstanding, effective means of automatically extracting interesting musical information from a sea of redundant data.

  7. Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction. (United States)

    Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim


    The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (Pextraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

  8. Stability analysis of underground openings for extraction of natural stone

    Directory of Open Access Journals (Sweden)

    Karmen Fifer Bizjak


    Full Text Available Extraction of natural stone is usually carried out in surface quarries. Underground excavation is not a frequently used method. Due to the restrictive environmental legislature and limited stores of natural stone, underground extraction has become quite an interestingalternative. Dimensions of underground openings are determined with stability analyses.Prior to starting a numerical analysis of a large underground opening it is very important to determine the mechanism of failure and set up a proper numerical model. The continuum method is usually used in rock mechanics. A disadvantage of this calculation is that it cannotbe applied to a large number of joints. Other methods are preferred, such as the numerical discrete method, which allows joint systems to be involved into calculations. The most probable failure of rock with several joint systems is block sliding. In the example of themarble of Hotavlje both methods were used. It was established that the continuum method is convenient for the global stability prediction of the underground opening. Further discretemethod enable the block stability calculation. The analytical block analysis is still accurate for the a stability calculation of single block. The prerequisite for a good numerical analysis is sufficient quality data on geomechanical properties of rock. In-situ tests, laboratory tests and geotechnical measurements on the site are therefore necessary. Optimum dimensions of underground chambers in the Quarry of Hotavlje were calculated by using several numericalmodels, and the maximum chamber width of 12 m was obtained.

  9. Analysis of a novel field dilution method for testing samples that exceed the analytic range of point-of-care blood lead analyzers. (United States)

    Neri, Antonio James; Roy, Joannie; Jarrett, Jeffery; Pan, Yi; Dooyema, Carrie; Caldwell, Kathleen; Umar-Tsafe, Nasir Tsafe; Olubiyo, Ruth; Brown, Mary Jean


    Investigators developed and evaluated a dilution method for the LeadCare II analyzer (LCII) for blood lead levels >65 μg/dL, the analyzer's maximum reporting value. Venous blood samples from lead-poisoned children were initially analyzed in the field using the dilution method. Split samples were analyzed at the US Centers for Disease Control and Prevention (CDC) laboratory using both the dilution method and inductively coupled plasma-mass spectrometry (ICP-MS). The concordance correlation coefficient of CDC LCII vs. ICP-MS values (N = 211) was 0.976 (95 % confidence interval (CI) 0.970-0.981); of Field LCII vs. ICP-MS (N = 68) was 0.910 (95% CI 0.861-0.942), and CDC LCII vs. Field LCII (N = 53) was 0.721 (95% CI 0.565-0.827). Sixty percent of CDC and 54% of Field LCII values were within ±10% of the ICP-MS value. Results from the dilution method approximated ICP-MS values and were useful for field-based decision-making. Specific recommendations for additional evaluation are provided.

  10. Determination of urea kinetics by isotope dilution with [C-13]urea and gas chromatography isotope ratio mass spectrometry (GC-IRMS) analysis

    NARCIS (Netherlands)

    Kloppenburg, Wybe; Wolthers, BG; Stellaard, F; Elzinga, H; Tepper, T; deJong, PE; Huisman, RM


    1. Stable urea isotopes can be used to study urea kinetics in humans, The use of stable urea isotopes far studying urea kinetic parameters in humans on a large scale is hampered by the high costs of the labelled material, We devised a urea dilution for measurement of the distribution volume, product

  11. Extraction of glabridin with heat reflux extraction by response surface analysis

    Directory of Open Access Journals (Sweden)

    Li-ying DING


    Full Text Available Objective: To study the extraction process of glabridin from Glycyrrhiza glabra. Methods: The solid-liquid ratio, extraction time and extraction temperature are the three main factors in the experiment, and the extract solvent is ethyl acetate. Establish the response surface quadratic regression equation of glabridin extraction rate and purity. Results:The results indicate that the optimum conditions for glabridin are as follows: solvent is ethyl acetate, extraction time is 90 min, the ratio of solvent to solid is 35 ∶1 (ml/g, and extraction temperature is 44.7 ℃, purity and the maximum yield of Extraction of glabridin are 6.96% and 0.241%, The validation test shows that the experimental values of the model are 0.235% and 6.05% . Conclusion: The model equation can predict the experimental results, it can be used as reference in industrial production. 

  12. Observation and analysis of the diluted water and red tide in the sea off the Changjiang River mouth in middle and late June 2003

    Institute of Scientific and Technical Information of China (English)

    ZHU Jianrong; WANG Jinhui; SHEN Huanting; WU Hui


    An interdisciplinary comprehensive survey was conducted in middle and late June 2003 with the Multi- Parameter Environmental Monitoring System YSI6600 and water sample analysis in the sea off the Changjiang River mouth. The Changjiang diluted water (CDW) extended offshore with a bimodal structure during the observation, one extending toward the southeast, the other toward the northeast. The main axis of the CDW extended toward the northeast. A severe red tide with wide spatial extent and brown water color happened. Chlorophyll-a (Chl-a) distribution near the Changjiang River mouth also presented a bimodal structure, and its position and shape were roughly consistent with the extension of the CDW. Water sample analysis indicated that the serious eutrophication produced by the huge amount of nutrient load via the Changjiang River was the main cause of red tide bloom. The dominant algal specie at the most measurement stations was skeletonema costatum. There existed three centers of higher Chl-a concentration, locating at (122.45°E, 31.5°N), (122.4°E, 30.8°N) and (123.25°E, 30.0°N), respectively. The red tide at (122.45°E, 31.5°N) was located in the major modal of CDW and higher turbid seawater, its dominant algal specie was prorocentrum dentatum with density 2.23×106 ind/L. The red tide at (122.4°E, 30.8°N) was located in the second modal of CDW and lower turbid seawater, its dominant algal specie was skeletonema costatum with density 1.0×107 ind/L. The dominant algal specie at (123.25°E, 30.0°N) was Heterocapsa circularisquama horiguchi with density 2.0×106 ind/L, which was found for the first time forming red tide in the sea off the Changjiang River mouth.

  13. Lowering detection limits for 1,2,3-trichloropropane in water using solid phase extraction coupled to purge and trap sample introduction in an isotope dilution GC-MS method. (United States)

    Liao, Wenta; Ghabour, Miriam; Draper, William M; Chandrasena, Esala


    Purge and trap sample introduction (PTI) has been the premier sampling and preconcentration technique for gas chromatographic determination of volatile organic compounds (VOCs) in drinking water for almost 50 years. PTI affords sub parts-per-billion (ppb) detection limits for purgeable VOCs including fixed gases and higher boiling hydrocarbons and halocarbons. In this study the coupling of solid phase extraction (SPE) to PTI was investigated as a means to substantially increase enrichment and lower detection limits for the emerging contaminant, 1,2,3-trichloropropane (TCP). Water samples (500 mL) were dechlorinated, preserved with a biocide, and spiked with the isotope labeled internal standard, d5-TCP. The entire 500 mL sample was extracted with activated carbon or carbon molecular sieve SPE cartridges, and then eluted with dichloromethane -- excess solvent was removed in a nitrogen evaporator and diethylene glycol "keeper" remaining was dispersed in 5 mL of water for PTI GC-MS analysis. The experimental Method Detection Limit (MDL) for TCP was 0.11 ng/L (ppt) and accuracy was 95-103% in sub-ppt determinations. Groundwater samples including impaired California sources and treated water (n = 21) were analyzed with results ranging from below the method reporting limit (0.30 ng/L) to > 250 ng/L. Coupling of SPE with PTI may provide similar reductions in detection limits for other VOCs with appropriate physical-chemical properties.

  14. Toxicity of contaminated sediments in dilution series with control sediments (United States)

    Nelson, M.K.; Landrum, P.F.; Burton, G.A.; Klaine, S.J.; Crecelius, E.A.; Byl, T.D.; Gossiaux, Duane C.; Tsymbal, V.N.; Cleveland, L.; Ingersoll, Christopher G.; Sasson-Brickson, G.


    The use of dilutions has been the foundation of our approach for assessing contaminated water, and accordingly, it may be important to establish similar or parallel approaches for sediment dilutions. Test organism responses to dilution gradients can identify the degree of necessary sediment alteration to reduce the toxicity. Using whole sediment dilutions to represent the complex interactions of in situ sediments can identify the toxicity, but the selection of the appropriate diluent for the contaminated sediment may affect the results and conclusions drawn. Contaminated whole sediments were examined to evaluate the toxicity of dilutions of sediments with a diversity of test organisms. Dilutions of the contaminated sediments were prepared with differing diluents that varied in organic carbon content, particle size distribution, and volatile solids. Studies were conducted using four macroinvertebrates and a vascular, rooted plant. Responses by some test organisms followed a sigmoidal dose-response curve, but others followed a U-shaped curve. Initial dilutions reduced toxicity as expected, but further dilution resulted in an increase in toxicity. The type of diluent used was an important factor in assessing the sediment toxicity, because the control soil reduced toxicity more effectively than sand as a diluent of the same sediment. Using sediment chemical and physical characteristics as an indicator of sediment dilution may not be as useful as chemical analysis of contaminants, but warrants further investigation.

  15. Data Clustering Analysis Based on Wavelet Feature Extraction

    Institute of Scientific and Technical Information of China (English)

    QIANYuntao; TANGYuanyan


    A novel wavelet-based data clustering method is presented in this paper, which includes wavelet feature extraction and cluster growing algorithm. Wavelet transform can provide rich and diversified information for representing the global and local inherent structures of dataset. therefore, it is a very powerful tool for clustering feature extraction. As an unsupervised classification, the target of clustering analysis is dependent on the specific clustering criteria. Several criteria that should be con-sidered for general-purpose clustering algorithm are pro-posed. And the cluster growing algorithm is also con-structed to connect clustering criteria with wavelet fea-tures. Compared with other popular clustering methods,our clustering approach provides multi-resolution cluster-ing results,needs few prior parameters, correctly deals with irregularly shaped clusters, and is insensitive to noises and outliers. As this wavelet-based clustering method isaimed at solving two-dimensional data clustering prob-lem, for high-dimensional datasets, self-organizing mapand U-matrlx method are applied to transform them intotwo-dimensional Euclidean space, so that high-dimensional data clustering analysis,Results on some sim-ulated data and standard test data are reported to illus-trate the power of our method.

  16. Extraction, chromatographic and mass spectrometric methods for lipid analysis. (United States)

    Pati, Sumitra; Nie, Ben; Arnold, Robert D; Cummings, Brian S


    Lipids make up a diverse subset of biomolecules that are responsible for mediating a variety of structural and functional properties as well as modulating cellular functions such as trafficking, regulation of membrane proteins and subcellular compartmentalization. In particular, phospholipids are the main constituents of biological membranes and play major roles in cellular processes like transmembrane signaling and structural dynamics. The chemical and structural variety of lipids makes analysis using a single experimental approach quite challenging. Research in the field relies on the use of multiple techniques to detect and quantify components of cellular lipidomes as well as determine structural features and cellular organization. Understanding these features can allow researchers to elucidate the biochemical mechanisms by which lipid-lipid and/or lipid-protein interactions take place within the conditions of study. Herein, we provide an overview of essential methods for the examination of lipids, including extraction methods, chromatographic techniques and approaches for mass spectrometric analysis.

  17. Quantitative spatial analysis of the mouse brain lipidome by pressurized liquid extraction surface analysis

    DEFF Research Database (Denmark)

    Almeida, Reinaldo; Berzina, Zane; Christensen, Eva Arnspang


    of internal lipid standards in the extraction solvent. The analysis of lipid microextracts by nanoelectrospray ionization provides long-lasting ion spray which in conjunction with a hybrid ion trap-orbitrap mass spectrometer enables identification and quantification of molecular lipid species using a method......Here we describe a novel surface sampling technique termed pressurized liquid extraction surface analysis (PLESA), which in combination with a dedicated high-resolution shotgun lipidomics routine enables both quantification and in-depth structural characterization of molecular lipid species...... with successive polarity shifting, high-resolution Fourier transform mass spectrometry (FTMS), and fragmentation analysis. We benchmarked the performance of the PLESA approach for in-depth lipidome analysis by comparing it to conventional lipid extraction of excised tissue homogenates and by mapping the spatial...

  18. Extracting Metallic Nanoparticles from Soils for Quantitative Analysis: Method Development Using Engineered Silver Nanoparticles and SP-ICP-MS. (United States)

    Schwertfeger, D M; Velicogna, Jessica R; Jesmer, Alexander H; Saatcioglu, Selin; McShane, Heather; Scroggins, Richard P; Princz, Juliska I


    The lack of an efficient and standardized method to disperse soil particles and quantitatively subsample the nanoparticulate fraction for characterization analyses is hindering progress in assessing the fate and toxicity of metallic engineered nanomaterials in the soil environment. This study investigates various soil extraction and extract preparation techniques for their ability to remove nanoparticulate Ag from a field soil amended with biosolids contaminated with engineered silver nanoparticles (AgNPs), while presenting a suitable suspension for quantitative single-particle inductively coupled plasma mass spectroscopy (SP-ICP-MS) analysis. Extraction parameters investigated included reagent type (water, NaNO3, KNO3, tetrasodium pyrophosphate (TSPP), tetramethylammonium hydroxide (TMAH)), soil-to-reagent ratio, homogenization techniques as well as procedures commonly used to separate nanoparticles from larger colloids prior to analysis (filtration, centrifugation, and sedimentation). We assessed the efficacy of the extraction procedure by testing for the occurrence of potential procedural artifacts (dissolution, agglomeration) using a dissolved/particulate Ag mass ratio and by monitoring the amount of Ag mass in discrete particles. The optimal method employed 2.5 mM TSPP used in a 1:100 (m/v) soil-to-reagent ratio, with ultrasonication to enhance particle dispersion and sedimentation to settle out the micrometer-sized particles. A spiked-sample recovery analysis shows that 96% ± 2% of the total Ag mass added as engineered AgNP is recovered, which includes the recovery of 84.1% of the particles added, while particle recovery in a spiked method blank is ∼100%, indicating that both the extraction and settling procedure have a minimal effect on driving transformation processes. A soil dilution experiment showed that the method extracted a consistent proportion of nanoparticulate Ag (9.2% ± 1.4% of the total Ag) in samples containing 100%, 50%, 25%, and 10

  19. Dilution Methods in Flow Injection Analysis. Evaluation of Different Approaches as Exemplified for the Determination of Nitrosyl in Concentrated Sulphuric Acid

    DEFF Research Database (Denmark)

    Jørgensen, Ulla Vang; Nielsen, Steffen; Hansen, Elo Harald


    Instigated by developing a flow injection procedure for assay of nitrosyl in concentrated sulphuric acid, different approaches for reliable and robust on-line dilution in FIA were evaluated. These comprised the application of mixing tees in conjunction with mixing coils (including knotted reactors...... approach the criteria stipulated were that the procedure should allow a dilution factor of approximately 100, yet without excessive zone spreading, so that it, on one hand, effectively could eliminate the pronounced Schlieren effect encountered when mixing concentrated sulphuric acid with an aqueous...... in conjunction with knotted reactors of relatively large internal diameter (1.5 mm). The optimized FI-manifold was used with the Griess method for the spectrophotometric assay of nitrosyl (nitrite) in standards prepared in the matrix of concentrated sulphuric acid (detection limit 0.16 mg/l NO+-N (3s...

  20. Antibacterial effect of several extracts of Dictyophora indusiata to bacteria common in food determined by micro-broth dilution method%微量肉汤稀释法测定长裙竹荪多种提取物对食品中常见细菌的抑制效果

    Institute of Scientific and Technical Information of China (English)

    曹奕; 孙晓红; 陈燕; 赵勇; Vivian C H Wu; 潘迎捷


    Dictyophora indusiata was chosen as the sample, got the volatile oil with hydro-distillation after soxlet extracting,and the extracts extracted by ethanol.n-butanol and petroleum ether at the same time.With the micro broth dilution method,got the MIC values of all kinds of extracts to eight kinds of bacteria common in food,as the indicators to evaluate the antibacterial effect.Results showed that the antibacterial effect of volatile oils were better than three kinds of organic solvent extract in the culture medium. By comparison of results with colonial counting and research results of others at the same time,proving the micro broth dilution method as a determination method with feasibility and accuracy.%选取长裙竹荪为样品,采用索氏抽提后水蒸馏萃取获得挥发油,同时分别以乙醇、正丁醇、石油醚等有机溶剂萃取得到相应提取物.以8种食品中常见细菌为供试对象,由微量肉汤稀释法测得各类提取物对其的MIC值,作为评价其抑菌效果的指标结果表明:纯培养环境下,挥发油的抑菌效果优于三种有机溶剂提取物.通过与平板涂布计数结果及其它方法比较分析,进一步证明肉汤稀释法作为测定抑菌效果所具有的优越性.

  1. Quantity and unit extraction for scientific and technical intelligence analysis (United States)

    David, Peter; Hawes, Timothy


    Scientific and Technical (S and T) intelligence analysts consume huge amounts of data to understand how scientific progress and engineering efforts affect current and future military capabilities. One of the most important types of information S and T analysts exploit is the quantities discussed in their source material. Frequencies, ranges, size, weight, power, and numerous other properties and measurements describing the performance characteristics of systems and the engineering constraints that define them must be culled from source documents before quantified analysis can begin. Automating the process of finding and extracting the relevant quantities from a wide range of S and T documents is difficult because information about quantities and their units is often contained in unstructured text with ad hoc conventions used to convey their meaning. Currently, even simple tasks, such as searching for documents discussing RF frequencies in a band of interest, is a labor intensive and error prone process. This research addresses the challenges facing development of a document processing capability that extracts quantities and units from S and T data, and how Natural Language Processing algorithms can be used to overcome these challenges.

  2. Object-based Analysis for Extraction of Dominant Tree Species

    Institute of Scientific and Technical Information of China (English)

    Meiyun; SHAO; Xia; JING; Lu; WANG


    As forest is of great significance for our whole development and the sustainable plan is so focus on it. It is very urgent for us to have the whole distribution,stock volume and other related information about that. So the forest inventory program is on our schedule. Aiming at dealing with the problem in extraction of dominant tree species,we tested the highly hot method-object-based analysis. Based on the ALOS image data,we combined multi-resolution in e Cognition software and fuzzy classification algorithm. Through analyzing the segmentation results,we basically extract the spruce,the pine,the birch and the oak of the study area. Both the spectral and spatial characteristics were derived from those objects,and with the help of GLCM,we got the differences of each species. We use confusion matrix to do the Classification accuracy assessment compared with the actual ground data and this method showed a comparatively good precision as 87% with the kappa coefficient 0. 837.

  3. Determining the best extractant and extraction conditions for fulvic acid through qualitative and quantitative analysis of vermicompost

    Directory of Open Access Journals (Sweden)

    Omid Shabnani Moghadam


    Full Text Available Fulvic acid is a natural tampon and an appropriate chelating agent that has high ion-exchange ability and increasing absorption of minerals in plants. This paper examined the effects of extractants (sodium hydroxide, sodium polyphosphate, urea and EDTA and the extraction time (1, 7 and 9 days on the physicochemical properties of vermicompost-produced fulvic acid. Finally, various methods were compared to the universal method of humic substances. Different qualitative and quantitative analysis such as detecting the functional groups (FTIR, measurement of functional groups, spectrophotometric ratios and humification indices were carried out on fulvic acid. Results showed that the highest and lowest amounts of fulvic acid were extracted by the sodium hydroxide and urea, respectively. Various extractants made negligible changes in the type and quality of the Fulvic acid functional groups. Results indicated that sodium hydroxide was the best extractant and the minimum amounts of fulvic acid were extracted by the urea. Urea-extracted fulvic acid had the most functional groups of total acidity and phenolic OH. The most carboxyl functional groups and spectrophotometric ratios were detected in EDTA solution. At the end, by the comparison of various methods, universal method despite the low extraction amount had more functional groups and higher efficiencies compare to others.

  4. Extracting Credible Dependencies for Averaged One-Dependence Estimator Analysis

    Directory of Open Access Journals (Sweden)

    LiMin Wang


    Full Text Available Of the numerous proposals to improve the accuracy of naive Bayes (NB by weakening the conditional independence assumption, averaged one-dependence estimator (AODE demonstrates remarkable zero-one loss performance. However, indiscriminate superparent attributes will bring both considerable computational cost and negative effect on classification accuracy. In this paper, to extract the most credible dependencies we present a new type of seminaive Bayesian operation, which selects superparent attributes by building maximum weighted spanning tree and removes highly correlated children attributes by functional dependency and canonical cover analysis. Our extensive experimental comparison on UCI data sets shows that this operation efficiently identifies possible superparent attributes at training time and eliminates redundant children attributes at classification time.

  5. Blind extraction of an exoplanetary spectrum through Independent Component Analysis

    CERN Document Server

    Waldmann, Ingo P; Deroo, Pieter; Hollis, Morgan D J; Yurchenko, Sergey N; Tennyson, Jonathan


    Blind-source separation techniques are used to extract the transmission spectrum of the hot-Jupiter HD189733b recorded by the Hubble/NICMOS instrument. Such a 'blind' analysis of the data is based on the concept of independent component analysis. The de-trending of Hubble/NICMOS data using the sole assumption that nongaussian systematic noise is statistically independent from the desired light-curve signals is presented. By not assuming any prior, nor auxiliary information but the data themselves, it is shown that spectroscopic errors only about 10 - 30% larger than parametric methods can be obtained for 11 spectral bins with bin sizes of ~0.09 microns. This represents a reasonable trade-off between a higher degree of objectivity for the non-parametric methods and smaller standard errors for the parametric de-trending. Results are discussed in the light of previous analyses published in the literature. The fact that three very different analysis techniques yield comparable spectra is a strong indication of th...


    Energy Technology Data Exchange (ETDEWEB)

    Waldmann, I. P.; Tinetti, G.; Hollis, M. D. J.; Yurchenko, S. N.; Tennyson, J. [Department of Physics and Astronomy, University College London, Gower Street, WC1E 6BT (United Kingdom); Deroo, P., E-mail: [Jet Propulsion Laboratory, California Institute of Technology, 4800 Oak Grove Drive, Pasadena, CA 91109-8099 (United States)


    Blind-source separation techniques are used to extract the transmission spectrum of the hot-Jupiter HD189733b recorded by the Hubble/NICMOS instrument. Such a 'blind' analysis of the data is based on the concept of independent component analysis. The detrending of Hubble/NICMOS data using the sole assumption that nongaussian systematic noise is statistically independent from the desired light-curve signals is presented. By not assuming any prior or auxiliary information but the data themselves, it is shown that spectroscopic errors only about 10%-30% larger than parametric methods can be obtained for 11 spectral bins with bin sizes of {approx}0.09 {mu}m. This represents a reasonable trade-off between a higher degree of objectivity for the non-parametric methods and smaller standard errors for the parametric de-trending. Results are discussed in light of previous analyses published in the literature. The fact that three very different analysis techniques yield comparable spectra is a strong indication of the stability of these results.

  7. 分散固相萃取-同位素稀释高分辨质谱法测定植物油中16种邻苯二甲酸酯%Determination of 16 phthalate esters in vegetable oils by dispersive solid phase extraction-high resolution mass spectrometry with isotope dilution technique

    Institute of Scientific and Technical Information of China (English)

    陈达炜; 赵晓雪; 赵云峰; 苗虹


    目的:采用高效液相色谱-四级杆/静电场轨道阱高分辨质谱建立分散固相萃取法(dispersive solid phase extraction, d-SPE)快速分析植物油中16种邻苯二甲酸酯(Phthalate esters, PAEs)的检测方法。方法样品采用正己烷饱和的乙腈提取,经N-丙基乙二胺(primary secondary amine, PSA)和Nano Carb填料分散固相萃取净化,以BEH phenyl色谱柱为分析柱,0.1%甲酸乙腈及0.1%甲酸水溶液作为流动相进行梯度洗脱分离。采用正离子采集模式对植物油样品进行快速筛查,并对16种PAEs进行定量测定。结果16种PAEs在2~500μg/L范围内呈良好的线性关系,回归系数(r)大于0.995,该方法的定量限为8~10μg/kg。在不同加标水平下的平均回收率为77.9%~115.6%,相对标准偏差为0.3%~8.9%。结论本方法简单、灵敏、准确,适用于植物油中PAEs的快速筛查和定量测定。%Objective To establish a dispersive solid phase extraction (d-SPE)/high-resolution benchtop Q exactive mass spectrometry (HRMS) method for the rapid analysis of 16 phthalate esters (PAEs). Methods The samples were extracted with acetonitrile saturated with hexane, and cleaned up by d-SPE with the N-propyl ethlene diamine (PSA) and Nano Carb as the sorbents. The chromatographic analysis was performed on a BEH phenyl column with 0.1%formic acid in acetonitrile and 0.1%formic acid solution as the mobile phase and a gradient elution program was used. The PAEs were analyzed in positive mode by Q exactive high-resolution mass spectrometry, which were applied in rapid analysis of PAEs for vegetable oils. 16 PAEs analytes were screened qualitatively in the vegetable oil samples and then quantified by isotope dilution technique. Results All the target 16 PAEs showed a good linearity in the range of 2~500μg/L , and the aver-age recovery rates of the spiked vegetable oil samples were in the range of 77.9%~115.6%with the RSD in the range of 0.3%-8.9%. The limit of quantification (LOQ

  8. A Simplified Rice DNA Extraction Protocol for PCR Analysis

    Institute of Scientific and Technical Information of China (English)

    CHEN Wen-yue; CUI Hai-rui; BAO Jin-song; ZHOU Xiang-sheng; SHU Qing-yao


    A simple protocol was established for DNA extraction using etiolated rice seedlings, whereby rice DNA was directly extracted ir 0.5 mol/L NaOH solution in a single eppendorf tube. Results of comparative PCR analyses and electrophoresis showed that the DNA extracted using this method was as good and useful as that using standard CTAB method.

  9. Extraction and identification of flavonoids from parsley extracts by HPLC analysis (United States)

    Stan, M.; Soran, M. L.; Varodi, C.; Lung, I.


    Flavonoids are phenolic compounds isolated from a wide variety of plants, and are valuable for their multiple properties, including antioxidant and antimicrobial activities. In the present work, parsley (Petroselinum crispum L.) extracts were obtained by three different extraction techniques: maceration, ultrasonic-assisted and microwave-assisted solvent extractions. The extractions were performed with ethanol-water mixtures in various ratios. From these extracts, flavonoids like the flavones apigenin and luteolin, and the flavonols quercetin and kaempferol were identified using an HPLC Shimadzu apparatus equipped with PDA and MS detectors. The separation method involved a gradient step. The mobile phase consisted of two solvents: acetonitrile and distilled water with 0.1% formic acid. The separation was performed on a RP-C18 column.

  10. Instrument for Solvent Extraction and Analysis (ISEE) of Organics from Regolith Simulant Using Supercritical Fluid Extraction and Chromatography (United States)

    Franco, Carolina; Hintze, Paul E.


    ISEE is an instrument with the potential to perform extractions from regolith found on the surface of asteroids and planets, followed by characterization and quantitation of the extracts using supercritical fluid extraction (SFE) and chromatography (SFC). SFE is a developed technique proven to extract a wide range of organic compounds. SFC is similar to High Performance Liquid Chromatography (HPLC) but has the advantage of performing chiral separations without needing to derivatize the chiral compounds. CO2 will be the solvent for both stages as it is readily available in the Mars atmosphere. ISEE will capture CO2 from the environment, and use it for SFE and SFC. If successful, this would allow ISEE to perform analysis of organic compounds without using consumables. This paper will present results on a preliminary, proof-of-principle effort to use SFE and SFC to extract and analyze lunar regolith simulant spiked with organic compounds representing a range of organics that ISEE would expect to characterize. An optimization of variables for the extraction of the organics from the spiked regolith was successfully developed, using 138 bar pressure and 40 C temperature. The extraction flow rate was optimized at 2% SLPM with 30% methanol modifier. The extractions were successful with a value of 77.3+/- 0.9% of organics extracted. However, the recovery of organics after the extraction was very low with only 48.5+/-14.2%. Moreover, three columns were selected to analyze multiple samples at a time; two of them are Viridis HSS C18 SB and Torus DIOL, and the third column, specific for chiral separations, has not yet been selected yet.

  11. Extraction and analysis of polycyclic aromatic hydrocarbons (PAHs) by solid phase micro-extraction/supercritical fluid chromatography (SPME/SFC)

    Energy Technology Data Exchange (ETDEWEB)

    Lesellier, E. [Institut Universitaire de Technologie, (LETIAM), 91 - Orsay (France)


    Solid phase micro-extraction (SPME) is a clean and simple pre-concentration method. Previously used for trace analysis of volatile compounds, the use of SPME was extended to non volatile molecules with the development of an SPME/HPLC interface. This new interface allows the extraction and the analysis of high molecular weight compounds found in aqueous samples. Since superficial fluid chromatography is particularly well suited for analysis of complex mixtures containing non volatile compounds, the feasibility of coupling SPME and SFC has been investigated and applied to PAHs. Several points have been studied: behavior of interface and of fiber to superficial fluid and high pressure required by the analytical method; kind of the compounds transfer from the fiber to the analytical column; relation between the nature of the fibers and the quantity of extracted compounds; effect of salt addition. The results show that the SPME/SFC technic may be used for extraction and analysis of PAHs, since the quantity of extracted compounds reach 30 %. (author) 17 refs.

  12. Microwave-Assisted Extraction Followed by Solid-Phase Extraction for the Chromatographic Analysis of Alkaloids in Stephania cepharantha. (United States)

    Liu, Ying; Xie, Daotao; Kang, Yun; Wang, Yaqin; Yang, Ping; Guo, Jixian; Huang, Jianming


    A procedure involving microwave-assisted extraction (MAE) followed by solid-phase extraction (SPE) was established for the extraction and purification of three bisbenzylisoquinoline alkaloids from Stephania cepharantha, and a reversed-phase high-performance liquid chromatography (HPLC) method was developed for the quantification of the target alkaloids. Chromatographic separation was achieved on a Phenomenex Luna Phenyl-Hexyl column. Prior to the HPLC analysis, the alkaloids were rapidly extracted by an optimized MAE process using 0.01 mol/L hydrochloric acid as the solvent. The MAE extract was subsequently purified by SPE using a cation-exchange polymeric cartridge. The MAE-SPE procedure extracted the three alkaloids with satisfactory recoveries ranging from 100.44 to 102.12%. In comparison with the MAE, Soxhlet and ultrasonic-assisted extractions, the proposed MAE-SPE method showed satisfactory cleanup efficiency. Thus, the validated MAE-SPE-HPLC method is specific, accurate and applicable to the determination of alkaloids in S. cepharantha.

  13. Phosphogypsum analysis: total content and extractable element concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Gennari, Roseli F.; Medina, Nilberto H., E-mail:, E-mail: [Departamento de Fisica Nuclear, Instituto de Fisica (USP), Sao Paulo, SP (Brazil); Garcia, Isabella; Silveira, Marcilei A.G., E-mail: [Centro Universitario da FEI. Sao Bernardo do Campo, SP (Brazil)


    Phosphogypsum stand for the chemical origin gypsum generated in fertilizers production, in which phosphate rock is attacked by sulfuric acid resulting in phosphoric acid (H{sub 3}PO{sub 4}) and phosphate fertilizers. Phosphogypsum is not a commercial product and it is stocked in large open areas or accumulated in lakes inducing to a major environmental problem due to the presence of toxic and radioactive elements. The increasing world agricultural demand is the real responsible for the severity of this environmental problem. Nevertheless, there are some possibilities for the application of this reject material, such as civil construction, waste water treatment, and in cultivated lands, etc. In the agriculture the phosphogypsum is commonly used as a nutrient source due to its large amounts of phosphorus, calcium and sulfur. However, there are still some environmental questions related to the use of this by-product since phosphogypsum is classified as TENORM (Technologically Enhanced Naturally Occurring Radioactive Material), which is a solid waste containing heavy metals and naturally occurring radioactive elements from the rock matrix. In this work, Plasma Mass Spectrometry (ICP-MS) was used to study phosphogypsum samples. Several acid solutions for samples digestion were evaluated in order to be feasible the chemical analysis. BCR sequential extractions were also performed. The results showed analyte concentrations are highly dependent on the acid solution used. The BCR guidelines could not be applied as used for soil, since the phosphogypsum solubility is different. So, it would be necessary to use different mass aliquots in the extractions, to be feasible an environmental evaluation. (author)

  14. Generic on-line solid phase extraction sample preparation strategies for the analysis of drugs in biological matrices by LC-MS/MS. (United States)

    Bourgogne, Emmanuel; Grivet, Chantal; Varesio, Emmanuel; Hopfgartner, Gérard


    In the present work we investigate the integration of a single hardware platform (Prospekt-2) allowing on-line SPE with pre-/post-trapping dilution and direct injection of plasma extracts, and also compare the benefits and challenges of the different approaches for pharmaceutical drugs with heterogeneous physicochemical properties. In the first part, the generic use of on-line SPE with direct plasma injection or after protein precipitation was investigated for the quantitative analysis of talinolol. In the second part, pre-trapping and post-trapping dilution for on-line SPE is discussed for generic method development on an oxadiazole and its major metabolite. Finally, the difference of performance between direct plasma injection vs. off-line liquid-liquid extraction is also described for the quantification of buprenorphine and naltrexone down to 50 and 100 pg/ml using a 0.25 ml plasma aliquot. All assays were in human plasma and detection was performed by mass spectrometry detection either on simple or triple stage quadrupoles. Regardless of the tested strategy, assays were found linear, with precision and accuracy with <15% for all quality controls samples and <20% for lower limit of quantitation.

  15. Biodiversity inhibits parasites: Broad evidence for the dilution effect. (United States)

    Civitello, David J; Cohen, Jeremy; Fatima, Hiba; Halstead, Neal T; Liriano, Josue; McMahon, Taegan A; Ortega, C Nicole; Sauer, Erin Louise; Sehgal, Tanya; Young, Suzanne; Rohr, Jason R


    Infectious diseases of humans, wildlife, and domesticated species are increasing worldwide, driving the need to understand the mechanisms that shape outbreaks. Simultaneously, human activities are drastically reducing biodiversity. These concurrent patterns have prompted repeated suggestions that biodiversity and disease are linked. For example, the dilution effect hypothesis posits that these patterns are causally related; diverse host communities inhibit the spread of parasites via several mechanisms, such as by regulating populations of susceptible hosts or interfering with parasite transmission. However, the generality of the dilution effect hypothesis remains controversial, especially for zoonotic diseases of humans. Here we provide broad evidence that host diversity inhibits parasite abundance using a meta-analysis of 202 effect sizes on 61 parasite species. The magnitude of these effects was independent of host density, study design, and type and specialization of parasites, indicating that dilution was robust across all ecological contexts examined. However, the magnitude of dilution was more closely related to the frequency, rather than density, of focal host species. Importantly, observational studies overwhelmingly documented dilution effects, and there was also significant evidence for dilution effects of zoonotic parasites of humans. Thus, dilution effects occur commonly in nature, and they may modulate human disease risk. A second analysis identified similar effects of diversity in plant-herbivore systems. Thus, although there can be exceptions, our results indicate that biodiversity generally decreases parasitism and herbivory. Consequently, anthropogenic declines in biodiversity could increase human and wildlife diseases and decrease crop and forest production.

  16. Information- Theoretic Analysis for the Difficulty of Extracting Hidden Information

    Institute of Scientific and Technical Information of China (English)

    ZHANG Wei-ming; LI Shi-qu; CAO Jia; LIU Jiu-fen


    The difficulty of extracting hidden information,which is essentially a kind of secrecy, is analyzed by information-theoretic method. The relations between key rate, message rate, hiding capacity and difficulty of extraction are studied in the terms of unicity distance of stego-key, and the theoretic conclusion is used to analyze the actual extracting attack on Least Significant Bit(LSB) steganographic algorithms.

  17. Simultaneous extraction, optimization, and analysis of flavonoids and polyphenols from peach and pumpkin extracts using a TLC-densitometric method. (United States)

    Altemimi, Ammar; Watson, Dennis G; Kinsel, Mary; Lightfoot, David A


    The use of medicinal plants has been reported throughout human history. In the fight against illnesses, medicinal plants represent the primary health care system for 60 % of the world's population. Flavonoids are polyphenolic compounds with active anti-microbial properties; they are produced in plants as pigments. Quercetin, myricetin, and rutin are among the most well-known and prevalent flavonoids in plants, with an antioxidant activity capable of decreasing the oxidation of low density lipoproteins [LDLs]. To date, this research is the first of its kind to employ a coupled thin-layer chromatography (TLC) and a densitometric quantification method with a Box-Behnken design (BBD) response surface methodology (RSM) for optimization of ultrasonic-assisted extraction and determination of rutin and quercetin from peach and ellagic acid and myricetin from pumpkin fruits. The effect of process variables (extraction temperature (°C), extraction power (%) and extraction time (min)) on ultrasound-assisted extraction (UAE) were examined by using BBD and RSM. TLC followed by Quantity-One™ (BioRad) image analysis as a simple and rapid method was used for identification and quantification of the compounds in complex mixtures. The results were consistent under optimal conditions among the experimental values and their predicted values. A mass spectrometry (MALDI-TOF MS) technique was also used to confirm the identity of the natural products in the TLC spots resolved. The results show that the coupled TLC-densitometric methods & BBD can be a very powerful approach to qualitative and quantitative analysis of; rutin and quercetin from peach extracts; and ellagic acid and myricetin contents from pumpkin extracts.

  18. Comparative analysis of protocols for DNA extraction from soybean caterpillars. (United States)

    Palma, J; Valmorbida, I; da Costa, I F D; Guedes, J V C


    Genomic DNA extraction is crucial for molecular research, including diagnostic and genome characterization of different organisms. The aim of this study was to comparatively analyze protocols of DNA extraction based on cell lysis by sarcosyl, cetyltrimethylammonium bromide, and sodium dodecyl sulfate, and to determine the most efficient method applicable to soybean caterpillars. DNA was extracted from specimens of Chrysodeixis includens and Spodoptera eridania using the aforementioned three methods. DNA quantification was performed using spectrophotometry and high molecular weight DNA ladders. The purity of the extracted DNA was determined by calculating the A260/A280 ratio. Cost and time for each DNA extraction method were estimated and analyzed statistically. The amount of DNA extracted by these three methods was sufficient for PCR amplification. The sarcosyl method yielded DNA of higher purity, because it generated a clearer pellet without viscosity, and yielded high quality amplification products of the COI gene I. The sarcosyl method showed lower cost per extraction and did not differ from the other methods with respect to preparation times. Cell lysis by sarcosyl represents the best method for DNA extraction in terms of yield, quality, and cost effectiveness.

  19. An Automated Video Object Extraction System Based on Spatiotemporal Independent Component Analysis and Multiscale Segmentation

    Directory of Open Access Journals (Sweden)

    Zhang Xiao-Ping


    Full Text Available Video content analysis is essential for efficient and intelligent utilizations of vast multimedia databases over the Internet. In video sequences, object-based extraction techniques are important for content-based video processing in many applications. In this paper, a novel technique is developed to extract objects from video sequences based on spatiotemporal independent component analysis (stICA and multiscale analysis. The stICA is used to extract the preliminary source images containing moving objects in video sequences. The source image data obtained after stICA analysis are further processed using wavelet-based multiscale image segmentation and region detection techniques to improve the accuracy of the extracted object. An automated video object extraction system is developed based on these new techniques. Preliminary results demonstrate great potential for the new stICA and multiscale-segmentation-based object extraction system in content-based video processing applications.

  20. Cloud point extraction for trace inorganic arsenic speciation analysis in water samples by hydride generation atomic fluorescence spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li, Shan, E-mail:; Wang, Mei, E-mail:; Zhong, Yizhou, E-mail:; Zhang, Zehua, E-mail:; Yang, Bingyi, E-mail:


    A new cloud point extraction technique was established and used for the determination of trace inorganic arsenic species in water samples combined with hydride generation atomic fluorescence spectrometry (HGAFS). As(III) and As(V) were complexed with ammonium pyrrolidinedithiocarbamate and molybdate, respectively. The complexes were quantitatively extracted with the non-ionic surfactant (Triton X-114) by centrifugation. After addition of antifoam, the surfactant-rich phase containing As(III) was diluted with 5% HCl for HGAFS determination. For As(V) determination, 50% HCl was added to the surfactant-rich phase, and the mixture was placed in an ultrasonic bath at 70 °C for 30 min. As(V) was reduced to As(III) with thiourea–ascorbic acid solution, followed by HGAFS. Under the optimum conditions, limits of detection of 0.009 and 0.012 μg/L were obtained for As(III) and As(V), respectively. Concentration factors of 9.3 and 7.9, respectively, were obtained for a 50 mL sample. The precisions were 2.1% for As(III) and 2.3% for As(V). The proposed method was successfully used for the determination of trace As(III) and As(V) in water samples, with satisfactory recoveries. - Highlights: • Cloud point extraction was firstly established to determine trace inorganic arsenic(As) species combining with HGAFS. • Separate As(III) and As(V) determinations improve the accuracy. • Ultrasonic release of complexed As(V) enables complete As(V) reduction to As(III). • Direct HGAFS analysis can be performed.

  1. [DNA extraction methods of compost for molecular ecology analysis]. (United States)

    Yang, Zhao-Hui; Xiao, Yong; Zeng, Guang-Ming; Liu, Yun-Guo; Deng, Jiu-Hua


    Molecular ecology provides new techniques for studying compost microbes, and the DNA extraction is the basis of molecular techniques. Because of the contamination of humic acids, it turns to be more difficult for compost microbial DNA extraction. Three different approaches, named as lysozyme lysis, ultrasonic lysis and proteinase K lysis with CTAB, were used to extract the total DNA from compost. The detection performed on a nucleic acids and protein analyzer showed that all the three approaches produced high DNA yields. The agarose gel electrophoresis showed that the DNA fragments extracted from compost had a length of about 23 kb. A eubacterial 16S rRNA gene targeted primer pair (27F and 1 495R) was used for PCR amplification, and all the samples got almost the full length 16S rDNA sequence (about 1.5 kb). After digested by restriction endonucleases (Hae Ill and Alu I), the restriction map showed relatively identical microbial diversity in the DNA, which was extracted by the three different approaches. All the compost microbial DNA extracted by the three different approaches could be used for molecular ecological study, and researchers should choose the right approach for extracting microbial DNA from compost based on the facts.

  2. Landslide stability analysis on basis of LIDAR data extraction (United States)

    Hu, Hui; Fernandez-Steeger, Tomas M.; Dong, Mei; Azzam, Rafig


    important role during surface construction for further more precise analysis purpose. 3D geological model can be built based on the connection between surface model and geological data like borehole data in GOCAD. Regarding the bench stability analysis, LEM (Limit Equilibrium Method) analysis using Janbu and FEM (Finite Element Method) have been adopted during this analyzing task. A program was developed to convert GOCAD 2D section data directly into the FEM software. The meshed model is then used for stability analysis. In one quarry, 3 cross sections have been extracted on basis of LIDAR original data (original 3 cross sections). To evaluate the advantages of LIDAR data for slope analysis, the results of safety factor (SF) were compared to simplified slope models as they are used normally. The comparison showed that variations of the SF reach up to 9%. Additionally, conservative evaluation demonstrated by SF results based on simplified model is not adaptive for decision making of filling.

  3. Flavonoids content in extracts secang (Caesalpinia Sappan L.) maceration method infundation analysis and visible ultraviolet spectrophotometer

    National Research Council Canada - National Science Library

    Youstiana Dwi Rusita; Suhartono


    .... Analysis using univariate analysis. This study shows that there are types of flavonoids flavones, flavonols and flavanols on extracts of Caesalpinia sappan L results maceration method, and there are flavonoid types of flavones...

  4. In-Situ Liquid Extraction and Analysis Platform for Mars and Ocean Worlds (United States)

    Kehl, F.; Wu, D.; Mora, M. F.; Creamer, J. S.; Willis, P. A.


    We present a compact sample extractor and analysis unit, based on subcritical water extraction and flow injection analysis, that could be used to support robotic missions seeking chemical signatures of life on Mars, Europa, Enceladus or Titan.

  5. Cleanup and analysis of sugar phosphates in biological extracts by using solid phase extraction and anion-exchange chromatography with pulsed amperometric detection

    DEFF Research Database (Denmark)

    Smith, Hans Peter; Cohen, A.; Buttler, T.


    A cleanup method based on anion-exchange solid-phase extraction (SPE) was developed to render biological extracts suitable for the analysis of hexose phosphates with a modified anion-exchange chromatography method and pulsed amperometric detection. The method was applied to cell extracts of Sacch......A cleanup method based on anion-exchange solid-phase extraction (SPE) was developed to render biological extracts suitable for the analysis of hexose phosphates with a modified anion-exchange chromatography method and pulsed amperometric detection. The method was applied to cell extracts...... of Saccharomyces cerevisiae obtained by using cold methanol as quenching agent and chloroform as extraction solvent. It was shown that pretreatment of the cell extract with SPE markedly improved the quality of the liquid chromatography analysis with recoveries of the sugar phosphates close to 100%. Furthermore...

  6. The decision to extract: part II. Analysis of clinicians' stated reasons for extraction. (United States)

    Baumrind, S; Korn, E L; Boyd, R L; Maxwell, R


    In a recently reported study, the pretreatment records of each subject in a randomized clinical trial of 148 patients with Class I and Class II malocclusions presenting for orthodontic treatment were evaluated independently by five experienced clinicians (drawn from a panel of 14). The clinicians displayed a higher incidence of agreement with each other than had been expected with respect to the decision as to whether extraction was indicated in each specific case. To improve our understanding of how clinicians made their decisions on whether to extract or not, the records of a subset of 72 subjects randomly selected from the full sample of 148, have now been examined in greater detail. In 21 of these cases, all five clinicians decided to treat without extraction. Among the remaining 51 cases, there were 202 decisions to extract (31 unanimous decision cases and 20 split decision cases). The clinicians cited a total of 469 reasons to support these decisions. Crowding was cited as the first reason in 49% of decisions to extract, followed by incisor protrusion (14%), need for profile correction (8%), Class II severity (5%), and achievement of a stable result (5%). When all the reasons for extraction in each clinician's decision were considered as a group, crowding was cited in 73% of decisions, incisor protrusion in 35%, need for profile correction in 27%, Class II severity in 15% and posttreatment stability in 9%. Tooth size anomalies, midline deviations, reduced growth potential, severity of overjet, maintenance of existing profile, desire to close the bite, periodontal problems, and anticipation of poor cooperation accounted collectively for 12% of the first reasons and were mentioned in 54% of the decisions, implying that these considerations play a consequential, if secondary, role in the decision-making process. All other reasons taken together were mentioned in fewer than 20% of cases. In this sample at least, clinicians focused heavily on appearance

  7. Chemical Analysis and Biological Activity of Jordanian Chamomile Extracts

    Directory of Open Access Journals (Sweden)

    Nawal Hassan Al Bahtiti


    Full Text Available The Jordanian chamomile (Matricaria chamomilla has been researched more thoroughly to evaluate its useful properties. It is investigated and found that Jordanian chamomile is rich in phenolic compounds, with beneficial biological activities. By applying the most promising HPLC method, the content of total phenolics in methanolic extract was determined according to the Folin-Clocalteu procedure, and was found (GAE>20 mg/g. The flavonoid types were found as flavones and flavonolos.The minimum inhibitory concentration values for methanolic extracts of Jordanian chamomile were determined for different kinds of bacteria. The extracts have activity against Staphylococcus aurous, candida albicans, Esherichia Coli, Betula pubescens and Pinus sylvestris. The activity has been observed to be due to the tannins and a pigenin present in the extract. To utilize these significant sources of natural compounds, further characterization of phenolic composition is needed.

  8. [The extractive: life and death of an uncommon product of proximate analysis]. (United States)

    Tomic, Sacha


    Issued from the pharmaceutical tradition, the "extractive", formerly "extract", is a typical artefact of proximate analysis introduced in the new nomenclature of 1787. After beign one of its most active promotors, Fourcroy published with Vauquelin a posthumous paper in 1810 in which he expressed some doubts about the substance. Theoretically present in almost all vegetable extracts, some chemists, pharmacists and physicians try to isolate the extractive without success and instead accumulated contradictory results. At the end, the eviction of this chimaera held by sceptical chemists such as Chevreul and Braconnot and the conversion of other analysts, dismissed extractive and the name almost gradually disappears at the begining of the 1830s.

  9. Analysis of human muscle extracts by proton NMR

    Energy Technology Data Exchange (ETDEWEB)

    Venkatasubramanian, P.N.; Barany, M.; Arus, C.


    Perchloric acid extracts were prepared from pooled human muscle biopsies from patients diagnosed with scoliosis (SCOL) and cerebral palsy (CP). After neutralization with KOH and removal of perchlorate, the extracts were concentrated by freeze drying and dissolved in /sup 2/H/sub 2/O to contain 120 O.D. units at 280 nm per 0.5 ml. /sup 1/H NMR spectroscopy was performed with the 5 mm probe of a Varian XL300 instrument. Creatine, lactate, carnosine, and choline were the major resonances in the one-dimensional spectra of both extracts. With creatine as reference, 2.5-fold more lactate was found in SCOL than in CP, and a much smaller difference was also found in their carnosine content. Two-dimensional COSY comparison revealed several differences between the two extracts. Taurine, N-acetyl glutamate, glycerophosphoryl choline (or phosphoryl choline) and an unidentified spot were present only in the extract from SCOL but not in that from CP. On the other hand, aspartate, hydroxy-proline, carnitine and glycerophosphoryl ethanolamine were only present in CP but absent in SCOL. Alanine, cysteine, lysine and arginine appeared in both extracts without an apparent intensity difference.


    Energy Technology Data Exchange (ETDEWEB)

    Jones, M.; Diprete, D.; Wiedenman, B.


    The current mission at H-Canyon involves the dissolution of an Alternate Feedstocks 2 (AFS-2) inventory that contains plutonium metal. Once dissolved, HB-Line is tasked with purifying the plutonium solution via anion exchange, precipitating the Pu as oxalate, and calcining to form plutonium oxide (PuO{sub 2}). The PuO{sub 2} will provide feed product for the Mixed Oxide (MOX) Fuel Fabrication Facility, and the anion exchange raffinate will be transferred to H-Canyon. The results presented in this report document the potential success of the RE resin column extraction application on highly concentrated Pu samples to meet MOX feed product specifications. The original 'Hearts Cut' sample required a 10000x dilution to limit instrument drift on the ICP-MS method. The instrument dilution factors improved to 125x and 250x for the sample raffinate and sample eluent, respectively. As noted in the introduction, the significantly lower dilutions help to drop the total MRL for the analyte. Although the spike recoveries were half of expected in the eluent for several key elements, they were between 94-98% after Nd tracer correction. It is seen that the lower ICD limit requirements for the rare earths are attainable because of less dilution. Especially important is the extremely low Ga limit at 0.12 {mu}g/g Pu; an ICP-MS method is now available to accomplish this task on the sample raffinate. While B and V meet the column A limits, further development is needed to meet the column B limits. Even though V remained on the RE resin column, an analysis method is ready for investigation on the ICP-MS, but it does not mean that V cannot be measured on the ICP-ES at a low dilution to meet the column B limits. Furthermore, this column method can be applicable for ICP-ES as shown in Table 3-2, in that it trims the sample of Pu, decreasing and sometimes eliminating Pu spectral interferences.

  11. Analysis of PAHs in human serum using cloud point extraction and LC/MS

    Energy Technology Data Exchange (ETDEWEB)

    Sirimanne, S.R.; Ma, Li; McClure, C. [National Center for Health, Environmental Health and Lab. Sciences, Atlanta, GA (United States)


    In these laboratories, the authors assess human exposure to environmental toxicants by quantifying the levels of target toxicants in serum of exposed individuals. The levels of target analytes are often in trace levels and hence preconcentration and cleanup are prerequisites to the analysis of these trace toxicants. The authors have identified cloud point extraction as an impressive alternative to conventional solvent extraction due its beneficial properties and the greater extraction efficiencies. The authors report for the first time, extraction of PAHs from human serum using cloud point technology and analysis by HPLC.


    Institute of Scientific and Technical Information of China (English)

    Rong-shi Cheng; Yu-fang Shao; Ming-zhu Liu; Rong-qing Lu


    Careful measurements of the dilute solution viscosities of polyethylene glycol and polyvinyl alcohol in water were carried out. The reduced viscosities of both polymer solutions plot upward curves at extremely dilute concentration levels similar to the phenomena observed for many polymer solutions in the early 1950's. Upon observation of the changes of the flow times of pure water in and the wall surface wettability of the viscometer after measuring solution viscosity, a view was formed that the observed viscosity abnormality at extremely dilute concentration regions is solely due to the effect of adsorption of polymer chains onto the wall surface of viscometer. A theory of adsorption effect based on the Langmuir isotherms was proposed and a mathematical analysis for data treatment was performed. The theory could adequately describe the existing viscosity data. It seems necessary to correct the viscosity result of dilute polymer solutions measured by glass capillary viscometer by taking into account the effect of adsorption in all cases.

  13. Body composition by bioelectrical-impedance analysis compared with deuterium dilution and skinfold anthropometry in patients with chronic obstructive pulmonary disease

    Energy Technology Data Exchange (ETDEWEB)

    Schols, A.M.; Wouters, E.F.; Soeters, P.B.; Westerterp, K.R. (Univ. of Limburg, Maastricht (Netherlands))


    Body composition is an important measure of nutritional status in patients with chronic obstructive pulmonary disease (COPD). We generated a regression model for bioelectrical impedance (BI) by using deuterium dilution (2H2O) as a reference method in 32 COPD patients, aged 63 +/- 9 y (mean +/- SD), in stable pulmonary and cardiac condition. Height squared divided by resistance (Ht2/Res) correlated well with total body water (TBW) as measured by 2H2O (r = 0.93, P less than 0.001, SEE = 1.9 L). The best-fitting regression equation to predict TBW comprised Ht2/Res and body weight (r2 = 0.89, SEE = 1.8 L, P less than 0.001). BI-predicted TBW was used to estimate BI-fat-free mass (FFM) that was compared with skinfold-thickness-based FFM predictions (Anthr-FFM). Relative to BI-FFM a significant overestimation of 4.4 +/- 0.8 kg was found by Anthr-FFM. Our results suggest that BI is a useful measure of body composition in patients with severe COPD.

  14. Variability of Changjiang Diluted Water revealed by a 45-year long-term ocean hindcast and Self-Organizing Maps analysis (United States)

    Zeng, Xiangming; He, Ruoying; Zong, Haibo


    Based on long-term realistic ocean circulation hindcast for in the Bohai, Yellow, and East China Seas, 45 years (1961-2005) of sea surface salinity data were analyzed using Self-Organizing Maps (SOM) to have a better understanding of the Changjiang Diluted Water (CDW) variation. Three spatial patterns were revealed by the SOM: normal, transition, and extension. The normal pattern mainly occurs from December to May while the CDW hugs China's east coast closely and flows southward. The extension pattern is dominant from June to October when the CDW extends northwestward toward Jeju Island in an omega shape. The transition pattern prevails for the rest of the year. Pattern-averaged temperature, circulation, and chlorophyll-a concentration show significant differences. CDW area and its eastern most extension were explored as a function of the Changjiang runoff and regional upwelling index. We found that Changjiang runoff and upwelling index can be reasonable predictors for the overall CDW area, while ambient circulation determines the distribution and structure of the CDW, and thus the CDW eastern most extension.

  15. Magnetic analysis of a melt-spun Fe-dilute Cu{sub 60}Ag{sub 35}Fe{sub 5} alloy

    Energy Technology Data Exchange (ETDEWEB)

    Kondo, Shin-ichiro, E-mail: [Faculty of Engineering, Nagasaki University, 1-14 Bunkyo-machi, Nagasaki 852-8521 (Japan); Kaneko, Kazuhiro; Morimura, Takao; Nakashima, Hiromichi [Faculty of Engineering, Nagasaki University, 1-14 Bunkyo-machi, Nagasaki 852-8521 (Japan); Kobayashi, Shin-Taro; Michioka, Chishiro; Yoshimura, Kazuyoshi [Department of Chemistry, Kyoto University, Kitashirakawa Oiwake-cho, Sakyo-ku, Kyoto 606-8502 (Japan)


    The magnetic properties of a melt-spun Fe-dilute Cu{sub 60}Ag{sub 35}Fe{sub 5} alloy are examined by X-ray diffraction, magnetic measurements, and transmission electron microscopy (TEM). The X-ray diffraction patterns show that the as-spun and annealed (773 K×36 ks) samples contain Cu and Ag phases and no Fe phases; thus, most Fe atoms are dispersed as clusters. Magnetic measurements indicate that the as-spun and annealed samples exhibit superparamagnetic behavior at 300 K, whereas ferromagnetic and superparamagnetic behaviors coexist at 4.2 K. The magnetic moments of small clusters at 300 K are determined by the nonlinear least squares method as 5148 and 4671 μ{sub B} for as-spun and annealed samples, respectively, whereas those at 300 K are experimentally determined as 3500 and 3200 μ{sub B}. This decrease in magnetic moments may imply the formation of anti-ferromagnetic coupling by annealing. TEM observation of the melt-spun sample suggests that there are three regions with different compositions: Cu-rich, Ag-rich, and Fe-rich with no precipitation in the matrix. In addition, these regions have obscure interfaces. The magnetic clusters are attributed to the Fe-rich regions.

  16. A case study demonstrating analysis of stormflows, concentrations, and loads of nutrients in highway runoff and swale discharge with the Stochastic Empirical Loading and Dilution Model (SELDM) (United States)

    Granato, Gregory; Jones, Susan C.


    Decisionmakers need information about the quality and quantity of stormwater runoff, the risk for adverse effects of runoff on receiving waters, and the potential effectiveness of mitigation measures to reduce these risks. The Stochastic Empirical Loading and Dilution Model (SELDM) uses Monte Carlo methods to generate stormflows, concentrations, and loads from a highway site and an upstream basin to provide needed risk-based information. SELDM was designed to help inform water-management decisions for streams and lakes receiving runoff from a highway or other land-use site. The purpose of this paper is to provide a brief description of SELDM and a hypothetical case study demonstrating the type of risk-based information that SELDM can provide. Total nitrogen (TN) and total phosphorus (TP) were selected as example constituents because nutrients are a common concern throughout the Nation and data for receiving waters, highway runoff, and the performance of best management practices (BMPs) are readily available for these constituents. 

  17. Comparison of mineral trioxide aggregate and diluted formocresol in pulpotomized human primary molars: 42-month follow-up and survival analysis. (United States)

    Mettlach, Sarah E; Zealand, Cameron M; Botero, Tatiana M; Boynton, James R; Majewski, Robert F; Hu, Jan ChingChun


    The purpose of this study was to test the hypothesis that there is no significant difference in the clinical and radiographic outcomes of diluted formocresol (DFC) compared to gray mineral trioxide aggregate (GMTA) pulpotomy in human primary molars. A total of 152 children with 252 primary molars met selection criteria. Of those, 119 and 133 teeth were randomly assigned to the GMTA and DFC groups, respectively. Periapical radiographs, taken pre- and/or postoperatively and at each 6-month follow-up, were digitized and evaluated by three blinded and calibrated examiners. Over a 42-month period, a total of 865 clinical and radiographic evaluations were conducted. There was no significant difference in clinical success, with the cumulative proportion of GMTA-treated teeth surviving at 0.98 vs DFC-treated teeth at 0.95 (P>.05). Radiographic success, however, was significantly greater for GMTA vs DFC, with the cumulative proportion of GMTA-treated teeth surviving at 0.90 vs DFC-treated teeth at 0.47 (Pformocresol when used as a medicament for primary molar pulpotomies.

  18. GC-MS-olfactometric characterization of the most aroma-active components in a representative aromatic extract from Iranian saffron (Crocus sativus L.). (United States)

    Amanpour, Asghar; Sonmezdag, A Salih; Kelebek, Hasim; Selli, Serkan


    Aroma and aroma-active compounds of Iranian saffron (Crocus sativus L.) were analyzed by gas chromatography-mass spectrometry-olfactometry. The saffron aromatic extracts were obtained by four different extraction techniques including solvent-assisted flavour evaporation (SAFE), liquid-liquid extraction (LLE), solid phase extraction (SPE), and simultaneous distillation extraction (SDE) and compared to achieve a representative aromatic extract from saffron. According to sensory analysis, the aromatic extract obtained by SAFE was the most representative of saffron odour. A total of 28 aroma compounds were identified in saffron. Ketones were quantitatively the most dominant volatiles in saffron, followed by aldehydes and acids. Aroma extract dilution analysis (AEDA) was used for the determination of aroma-active compounds of saffron. A total of nine aroma-active compounds were detected in the aromatic extract. On the basis of the flavour dilution (FD) factor, the most powerful aroma active compounds were safranal (FD = 512), 4-ketoisophorone (FD = 256) and dihydrooxophorone (FD = 128).

  19. A review of the extraction and chromatographic determination methods for the analysis of parabens. (United States)

    Piao, Chunying; Chen, Ligang; Wang, Yu


    Parabens are a family of most widely used antimicrobial preservatives in food ingredients, cosmetic consumer products and pharmaceutical preparations. But several recent studies have cautioned that exposure to parabens may have more harmful consequences on animal and human health than what we realized previously, which made the analysis of parabens necessary. In this paper, we reviewed main sample preparation methods and chromatographic analysis methods proposed in formerly published works dealing with the analysis of parabens in different matrices. The sample preparation methods included ultrasonic assisted extraction, supercritical fluid extraction, pressurized liquid extraction, solid phase extraction, solid phase microextraction, liquid phase microextraction, dispersive liquid-liquid microextraction, stir bar sorptive extraction and matrix solid phase dispersion. The chromatographic analysis methods involved liquid chromatography, gas chromatography, and capillary electrophoresis. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Analysis of the Interactions of Botanical Extract Combinations Against the Viability of Prostate Cancer Cell Lines

    Directory of Open Access Journals (Sweden)

    Lynn S. Adams


    Full Text Available Herbal medicines are often combinations of botanical extracts that are assumed to have additive or synergistic effects. The purpose of this investigation was to compare the effect of individual botanical extracts with combinations of extracts on prostate cell viability. We then modeled the interactions between botanical extracts in combination isobolographically. Scutellaria baicalensis, Rabdosia rubescens, Panax-pseudo ginseng, Dendranthema morifolium, Glycyrrhiza uralensis and Serenoa repens were collected, taxonomically identified and extracts prepared. Effects of the extracts on cell viability were quantitated in prostate cell lines using a luminescent ATP cell viability assay. Combinations of two botanical extracts of the four most active extracts were tested in the 22Rv1 cell line and their interactions assessed using isobolographic analysis. Each extract significantly inhibited the proliferation of prostate cell lines in a time- and dose-dependent manner except repens. The most active extracts, baicalensis, D. morifolium, G. uralensis and R. rubescens were tested as two-extract combinations. baicalensis and D. morifolium when combined were additive with a trend toward synergy, whereas D. morifolium and R. rubescens together were additive. The remaining two-extract combinations showed antagonism. The four extracts together were significantly more effective than the two-by-two combinations and the individual extracts alone. Combining the four herbal extracts significantly enhanced their activity in the cell lines tested compared with extracts alone. The less predictable nature of the two-way combinations suggests a need for careful characterization of the effects of each individual herb based on their intended use.

  1. Determination of tributyltin (TBT) in marine sediment using pressurised liquid extraction-gas chromatography-isotope dilution mass spectrometry (PLE-GC-IDMS) with a hexane-tropolone mixture. (United States)

    Konieczka, Piotr; Sejerøe-Olsen, Berit; Linsinger, Thomas P J; Schimmel, Heinz


    Extraction conditions for the determination of tributyltin (TBT) in sediment samples have been developed further. The analytical procedure is based on spiking with isotopically labelled analyte, pressurised liquid extraction (PLE) with a hexane/tropolone mixture, Grignard derivatization and quantification by GC-MS. It was applied to two unknown sediment samples as part of an intercomparison exercise of the Comité Consultatif pour la Quantité de Matière (CCQM). The detection limit was approximately 1.5 ng/g TBT as Sn, while the repeatability and intermediate precision (as the coefficient of variation) were 1.9% and 3.2%, respectively. The expanded uncertainty was 6.2% (coverage factor k = 2), and the accuracy was confirmed by measurement of a certified reference material.

  2. Process optimization and analysis of microwave assisted extraction of pectin from dragon fruit peel. (United States)

    Thirugnanasambandham, K; Sivakumar, V; Prakash Maran, J


    Microwave assisted extraction (MAE) technique was employed for the extraction of pectin from dragon fruit peel. The extracting parameters were optimized by using four-variable-three-level Box-Behnken design (BBD) coupled with response surface methodology (RSM). RSM analysis indicated good correspondence between experimental and predicted values. 3D response surface plots were used to study the interactive effects of process variables on extraction of pectin. The optimum extraction conditions for the maximum yield of pectin were power of 400 W, temperature of 45 °C, extracting time of 20 min and solid-liquid ratio of 24 g/mL. Under these conditions, 7.5% of pectin was extracted. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Gas chromatography-mass spectrometry analysis of various organic extracts ofMerremia borneensisfrom Sabah

    Institute of Scientific and Technical Information of China (English)

    M Amzad Hossain; Muhammad Dawood Shah; Mahyar Sakari


    Objective:To analyse the chemical composition of different extracts ofMerremia borneensis (M. borneensis) by gas chromatography-mass spectrometry (GC-MS).Methods: The dried leaves powder was extracted with methanol at room temperature by using Soxhlet extractor. Methanol crude extracts ofM. borneensis were extrastel with hexane, chloroform, ethyl acetate and butanol. Results: Qualitative analyses of various organic crude extracts showed that majority of these are flavonoids, terpeniods, alkaloids and glycosides. Most of the identified compounds by GC-MS are biologically important. Further theM. borneensisleaf possesses certain characteristics that can be ascribed to cultivation on a domestic plantation.Conclusions: The suitable extracts for respective compounds can be chosen on the basis of aboveGC-MS analysis. All the major compounds from different extracts are biologically active molecules. Thus the identification of a good number of compounds from various extractsM. borneensis might have some ecological significance.

  4. Laminar Flame Velocity and Temperature Exponent of Diluted DME-Air Mixture (United States)

    Naseer Mohammed, Abdul; Anwar, Muzammil; Juhany, Khalid A.; Mohammad, Akram


    In this paper, the laminar flame velocity and temperature exponent diluted dimethyl ether (DME) air mixtures are reported. Laminar premixed mixture of DME-air with volumetric dilutions of carbon dioxides (CO2) and nitrogen (N2) are considered. Experiments were conducted using a preheated mesoscale high aspect-ratio diverging channel with inlet dimensions of 25 mm × 2 mm. In this method, flame velocities are extracted from planar flames that were stabilized near adiabatic conditions inside the channel. The flame velocities are then plotted against the ratio of mixture temperature and the initial reference temperature. A non-linear power law regression is observed suitable. This regression analysis gives the laminar flame velocity at the initial reference temperature and temperature exponent. Decrease in the laminar flame velocity and increase in temperature exponent is observed for CO2 and N2 diluted mixtures. The addition of CO2 has profound influence when compared to N2 addition on both flame velocity and temperature exponent. Numerical prediction of the similar mixture using a detailed reaction mechanism is obtained. The computational mechanism predicts higher magnitudes for laminar flame velocity and smaller magnitudes of temperature exponent compared to experimental data.

  5. Extraction of intracellular protein from Glaciozyma antarctica for proteomics analysis (United States)

    Faizura, S. Nor; Farahayu, K.; Faizal, A. B. Mohd; Asmahani, A. A. S.; Amir, R.; Nazalan, N.; Diba, A. B. Farah; Muhammad, M. Nor; Munir, A. M. Abdul


    Two preparation methods of crude extracts of psychrophilic yeast Glaciozyma antarctica were compared in order to obtain a good recovery of intracellular proteins. Extraction with mechanical procedures using sonication was found to be more effective for obtaining good yield compare to alkaline treatment method. The procedure is simple, rapid, and produce better yield. A total of 52 proteins were identified by combining both extraction methods. Most of the proteins identified in this study involves in the metabolic process including glycolysis pathway, pentose phosphate pathway, pyruyate decarboxylation and also urea cyle. Several chaperons were identified including probable cpr1-cyclophilin (peptidylprolyl isomerase), macrolide-binding protein fkbp12 and heat shock proteins which were postulate to accelerate proper protein folding. Characteristic of the fundamental cellular processes inferred from the expressed-proteome highlight the evolutionary and functional complexity existing in this domain of life.

  6. Thermal extraction analysis of five Los Azufres production wells

    Energy Technology Data Exchange (ETDEWEB)

    Kruger, Paul; Quijano, Luis


    Thermal energy extraction from five wells supplying 5-MWe wellhead generators in three zones of the Los Azufres geothermal field has been examined from production and chemical data compiled over 14-years of operation. The data, as annual means, are useful in observing small-scale changes in reservoir performance with continuous production. The chemical components are chloride for quality control and the geothermometer elements for reservoir temperatures. The flowrate and fluid enthalpy data are used to calculate the thermal extraction rates. Integration of these data provides an estimate of the total energy extracted from the zone surrounding the well. The combined production and chemical geothermometer data are used to model the produced fluid as coming from just-penetrating wells for which the annual produced mass originates from a series of concentric hemispheric shells moving out into the reservoir. Estimates are made of the drawdown distance into the reservoir and the far-field conditions.

  7. Rapid method for the determination of 16 organochlorine pesticides in sesame seeds by microwave-assisted extraction and analysis of extracts by gas chromatography-mass spectrometry. (United States)

    Papadakis, Emmanouil N; Vryzas, Zisis; Papadopoulou-Mourkidou, Euphemia


    A method for the multiresidue analysis of 16 organochlorine insecticides in sesame seeds has been developed. The method is based on the microwave-assisted extraction (MAE) of the sesame seeds by the use of a water-acetonitrile mixture followed by Florisil clean-up of the extracts and subsequent analysis by gas chromatography-mass spectrometry (GC/MS) in the selected ion monitoring (SIM) mode. MAE operational parameters (extraction solvent, temperature and time, extractant volume) were optimized with respect to extraction efficiency of the target compounds from sesame seeds with 46% oil content. Recoveries >80% with relative standard deviations (RSD) seed samples imported to Greece.

  8. Phytochemical Analysis and Antioxidant Activity of Salvia chloroleuca Aerial Extracts (United States)

    Salimikia, Iraj; Reza Monsef-Esfahani, Hamid; Gohari, Ahmad Reza; Salek, Mehrnoosh


    Background Salvia, known as Maryam Goli in the Persian language, is an important genus that includes approximately 900 species in the Lamiaceae family. There are 58 Salvia species growing naturally in Iran, including Salvia chloroleuca Rech. f. and Allen., which grows wild in the northeastern and central parts of the country. Objectives This study was designed to determine the chemical composition, in vitro antioxidant activity, and total phenol content of various extracts of S. chloroleuca. Materials and Methods Dried aerial parts of the plant were crushed, then sequentially extracted with n-hexane, ethyl acetate, and methanol. The fractions of S. chloroleuca were subjected to silica gel column chromatography and Sephedex LH-20. The antioxidant activities of these extracts were measured by ferric reducing antioxidant power (FRAP), and the total phenolic contents of the extracts were evaluated using Folin-Ciocalteu reagent. Results The separation and purification processes were carried out using different chromatographic methods. Structural elucidation was on the basis 1H-NMR and 13C-NMR spectral data, in comparison with that reported in the literature. The isolated compounds were salvigenin (1), luteolin (2), cirsiliol (3), β-sitosterol (4), and daucosterol (5). Ethyl acetate extract displayed the highest level of total antioxidants and total polyphenols compared to the other analyzed extracts (n-hexane and methanol). In the FRAP assay, ethyl acetate extract had the highest (230.4±10.5) FRAP value, followed by methanol (211.4 ± 8.3) and n-hexane (143.4 ± 12.04). Total phenol contents were calculated to be 13.8 ± 0.3, 58.25 ± 0.05, and 43.48 ± 0.38 mg of gallic acid/100 g in the n-hexane, ethyl acetate, and methanol extracts, respectively. Conclusions The above-mentioned compounds were isolated for the first time from S. chloroleuca. The antioxidant activity of this plant could be in part related to isolated flavonoids and sterols. The results of this study

  9. Measuring the Soret coefficient of nanoparticles in a dilute suspension. (United States)

    Zhao, Chao; Fu, Jinxin; Oztekin, Alparslan; Cheng, Xuanhong


    Thermophoresis is an efficient process for the manipulation of molecules and nanoparticles due to the strong force it generates on the nanoscale. Thermophoresis is characterized by the Soret coefficient. Conventionally, the Soret coefficient of nanosized species is obtained by fitting the concentration profile under a temperature gradient at the steady state to a continuous phase model. However, when the number density of the target is ultralow and the dispersed species cannot be treated as a continuous phase, the bulk concentration fluctuates spatially, preventing extraction of temperature-gradient induced concentration profile. The present work demonstrates a strategy to tackle this problem by superimposing snapshots of nanoparticle distribution. The resulting image is suitable for the extraction of the Soret coefficient through the conventional data fitting method. The strategy is first tested through a discrete phase model that illustrates the spatial fluctuation of the nanoparticle concentration in a dilute suspension in response to the temperature gradient. By superimposing snapshots of the stochastic distribution, a thermophoretic depletion profile with low standard error is constructed, indicative of the Soret coefficient. Next, confocal analysis of nanoparticle distribution in response to a temperature gradient is performed using polystyrene nanobeads down to 1e-5% (v/v). The experimental results also reveal that superimposing enhances the accuracy of extracted Soret coefficient. The critical particle number density in the superimposed image for predicting the Soret coefficient is hypothesized to depend on the spatial resolution of the image. This study also demonstrates that the discrete phase model is an effective tool to study particle migration under thermophoresis in the liquid phase.

  10. Extraction, purification, methylation and GC-MS analysis of short-chain carboxylic acids for metabolic flux analysis. (United States)

    Tivendale, Nathan D; Jewett, Erin M; Hegeman, Adrian D; Cohen, Jerry D


    Dynamic metabolic flux analysis requires efficient and effective methods for extraction, purification and analysis of a plethora of naturally-occurring compounds. One area of metabolism that would be highly informative to study using metabolic flux analysis is the tricarboxylic acid (TCA) cycle, which consists of short-chain carboxylic acids. Here, we describe a newly-developed method for extraction, purification, derivatization and analysis of short-chain carboxylic acids involved in the TCA cycle. The method consists of snap-freezing the plant material, followed by maceration and a 12-15h extraction at -80 °C. The extracts are then subject to reduction (to stabilize β-keto acids), purified by strong anion exchange solid phase extraction and methylated with methanolic HCl. This method could also be readily adapted to quantify many other short-chain carboxylic acids.

  11. Rheological properties and orientational distributions of dilute ferromagnetic spherocylinder particle dispersions. Part II. Analysis for the two typical magnetic field directions. (United States)

    Aoshima, Masayuki; Satoh, Akira; Chantrell, Roy W; Coverdale, Geoff N


    We have investigated the orientational distributions and rheological properties of dilute colloidal dispersions, which consist of ferromagnetic spherocylinder particles. First, the governing equation of the orientational distribution function has been derived for the typical two cases of magnetic field directions: the direction parallel to the shear flow and the direction parallel to the angular velocity vector of the shear flow. The equation has been solved approximately by Galerkin's method. With these numerical solutions we have obtained the results of the orientational distribution and viscosity. The results obtained for the magnetic field in the shear flow direction are summarized as follows. In the case of a weak magnetic field, the particle tends to orient nearly toward the shear flow direction and its opposite direction. As the magnetic field increases, the orientation of the particle is restricted and the viscosity increases significantly. As the influence of the magnetic field becomes dominant, an overshoot in the viscosity curve appears. This is due to the fact that there is a maximum deviation of the averaged particle direction from the magnetic field direction. When the strength of the magnetic field increases significantly, the particle inclines close to the magnetic field direction and the viscosity converges to a constant value. Particles with a larger aspect ratio give rise to a larger increment in the viscosity since such elongated particles induce larger resistance in a flow field. We also have obtained results for the case of the magnetic field in the direction parallel to the angular velocity vector of the shear flow. When the flow field is dominant over both the rotational Brownian motion and the magnetic interaction, the particle rotates in the plane nearly perpendicular to the magnetic field direction. As the magnetic field increases, the particle inclines toward the magnetic direction. For this direction of field, the viscosity is

  12. Flavonoids content in extracts secang (Caesalpinia Sappan L. maceration method infundation analysis and visible ultraviolet spectrophotometer

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    Youstiana Dwi Rusita


    Full Text Available Secang (Caesalpinia sappan L has a component of a chemical compound essential oils, flavonoids, benzopyran, sapanin, brazilin, caesalpin S, caesalpin P, sapanon A, sapanon B. Flavonoids are chemical components that can be used in medical and industrial fields. This study aimed to determine the levels of flavonoids contained in extracts secang results maceration and extraction methods infundation. This study used quantitative and descriptive research design. This study using purposive sampling with two sample of Caesalpinia sappan L extract result of infundation and maceration. Analysis using univariate analysis. This study shows that there are types of flavonoids flavones, flavonols and flavanols on extracts of Caesalpinia sappan L results maceration method, and there are flavonoid types of flavones, flavonols and flavanols on extracts of Caesalpinia sappan L results infundation method. Flavonoid content test results showed that the levels of flavonoids in extracts of Caesalpinia sappan L results maceration 0.0539% whereas the levels of flavonoids in the extract of Caesalpinia sappan L results infundation methods 0.1902%. Necessary standardization of botanicals Caesalpinia sappan L to determine the levels of flavonoids using ultraviolet visible spectrophotometer, and the analysis of the levels of flavonoids in the extract of Caesalpinia sappan L using different solvents. As a follow-up is necessary to design the manufacture of dosage formulations of the active ingredient flavanoid compounds from the extract of Caesalpinia sappan L.

  13. Protective efficacy of Solanum xanthocarpum root extracts against free radical damage: phytochemical analysis and antioxidant effect. (United States)

    Kumar, S; Sharma, U K; Sharma, A K; Pandey, A K


    Free radicals have been implicated in many diseases. They attack biological macromolecules in healthy human cells and cause protein and DNA damage along with lipid peroxidation. Present study reports the phytochemical analysis as well as free radical scavenging and antioxidant activities of Solanum xanthocarpum root extracts. Tannins, flavonoids, terpenoids, alkaloids, saponins and steroids were present in different extracts. Total flavonoid content in extracts was quantified and maximum contents were found in ethyl acetate fraction followed by chloroform and ethyl alcohol fractions, respectively. Dose dependent response was observed in metal ion chelating activity of extracts. Comparatively better chelating activity was found in polar extracts. Most of the extracts exhibited significant free radical scavenging activity in DPPH radical scavenging assay. Ethanolic and aqueous extracts accounted for about 40—50% lipid peroxidation inhibition (LPOI) in rat liver homogenate. Antioxidant activity did not show direct correlation with the amount of flavonoid contents in the extracts. However, direct correlation was observed between DPPH free radical scavenging activity and LPOI. Antioxidant activity of the extracts was compared with standard antioxidants. The differential activity observed in extracts could be attributed to the presence of other phytochemicals such as tannins and terpenoids in addition to flavonoids. The study demonstrated appreciable protective efficacy in S. xanthocarpum root extracts against free radical damage.

  14. Acetonitrile extraction and dual-layer solid phase extraction clean-up for pesticide residue analysis in propolis. (United States)

    Oellig, Claudia


    Propolis is a very complex mixture of substances that is produced by honey bees and is known to be a rather challenging matrix for residue analysis. Besides resins, flavonoids and phenols, high amount of wax is co-extracted resulting in immense matrix effects. Therefore a suitable clean-up is crucial and indispensable. In this study, a reliable solid phase extraction (SPE) clean-up was developed for pesticide residue analysis in propolis. The clean-up success was quickly and easily monitored by high-performance thin-layer chromatography with different detection possibilities. The final method consists of the extraction of propolis with acetonitrile according to the QuEChERS method followed by an effective extract purification on dual-layer SPE cartridges with spherical hydrophobic polystyrene-divinylbenzene resin/primary secondary amine as sorbent and a mixture of toluene/acetone (95:5, v/v) for elution. Besides fat-soluble components like waxes, flavonoids, and terpenoids, more polar compounds like organic acids, fatty acids, sugars and anthocyanins were also removed to large extent. Method performance was assessed by recovery experiments at spiking levels of 0.5 and 1mg/kg (n=5) for fourteen pesticides that are relevant for propolis. Mean recoveries determined by HPLC-MS against solvent standards were between 40 and 101%, while calculation against matrix-matched standards provided recoveries of 79-104%. Precision of recovery, assessed by relative standard deviations, were below 9%. Thus, the developed dual-layer SPE clean-up enables the reliable pesticide residue analysis in propolis and provides a suitable alternative to time-consuming clean-up procedures proposed in literature.

  15. Local kernel nonparametric discriminant analysis for adaptive extraction of complex structures (United States)

    Li, Quanbao; Wei, Fajie; Zhou, Shenghan


    The linear discriminant analysis (LDA) is one of popular means for linear feature extraction. It usually performs well when the global data structure is consistent with the local data structure. Other frequently-used approaches of feature extraction usually require linear, independence, or large sample condition. However, in real world applications, these assumptions are not always satisfied or cannot be tested. In this paper, we introduce an adaptive method, local kernel nonparametric discriminant analysis (LKNDA), which integrates conventional discriminant analysis with nonparametric statistics. LKNDA is adept in identifying both complex nonlinear structures and the ad hoc rule. Six simulation cases demonstrate that LKNDA have both parametric and nonparametric algorithm advantages and higher classification accuracy. Quartic unilateral kernel function may provide better robustness of prediction than other functions. LKNDA gives an alternative solution for discriminant cases of complex nonlinear feature extraction or unknown feature extraction. At last, the application of LKNDA in the complex feature extraction of financial market activities is proposed.

  16. Evaluation of sample extraction methods for proteomics analysis of green algae Chlorella vulgaris. (United States)

    Gao, Yan; Lim, Teck Kwang; Lin, Qingsong; Li, Sam Fong Yau


    Many protein extraction methods have been developed for plant proteome analysis but information is limited on the optimal protein extraction method from algae species. This study evaluated four protein extraction methods, i.e. direct lysis buffer method, TCA-acetone method, phenol method, and phenol/TCA-acetone method, using green algae Chlorella vulgaris for proteome analysis. The data presented showed that phenol/TCA-acetone method was superior to the other three tested methods with regards to shotgun proteomics. Proteins identified using shotgun proteomics were validated using sequential window acquisition of all theoretical fragment-ion spectra (SWATH) technique. Additionally, SWATH provides protein quantitation information from different methods and protein abundance using different protein extraction methods was evaluated. These results highlight the importance of green algae protein extraction method for subsequent MS analysis and identification.

  17. User-oriented summary extraction for soccer video based on multimodal analysis (United States)

    Liu, Huayong; Jiang, Shanshan; He, Tingting


    An advanced user-oriented summary extraction method for soccer video is proposed in this work. Firstly, an algorithm of user-oriented summary extraction for soccer video is introduced. A novel approach that integrates multimodal analysis, such as extraction and analysis of the stadium features, moving object features, audio features and text features is introduced. By these features the semantic of the soccer video and the highlight mode are obtained. Then we can find the highlight position and put them together by highlight degrees to obtain the video summary. The experimental results for sports video of world cup soccer games indicate that multimodal analysis is effective for soccer video browsing and retrieval.

  18. Methodology of data extraction from a corpus for the conceptual analysis of metaphor in legal English


    Kucheruk, Liliya


    The present paper entitled “Methodology of data extraction from a corpus for the conceptual analysis of metaphor in legal English” investigates the main approaches to the study of metaphor in legal language from the point of view of cognitive linguistics. It also offers the most widely spread methods of data extraction form a corpus.


    Directory of Open Access Journals (Sweden)

    A. A. Chakhirova


    Full Text Available The article presents studies on development of cosmetics with complex extracts from herb of Bidens, flowers of Calendula, and flowers of Matricaria. We cited the analysis methods of the received extract and a drug on its base

  20. Analysis of heavy metals and fluoride in vegetation by extraction with concentrated mineral acids. (United States)

    Johnson, M S


    A rapid potentiometric method for determining fluoride in vegetation is described. Recovery of flouride by extraction with concentrated mineral acids compares favourably with standard methods of analysis in terms of accuracy and precision. The procedure affords the additional advantage that several citations are also quantitatively extracted and may be determined directly in the acid digest by atomic absorption spectrophotometry.

  1. Extraction and determination of molybdenum with tributyl phosphate Application to analysis of copper-molybdenum ores. (United States)

    Caiozzi, M; Zunino, H; Sepúlveda, L


    A differential spectrophotometric method is described for the determination of molybdenum by means of solvent extraction with tributylphosphate of the peroxymolybdate complex formed with H(2)O(2) in 3.5N H(2)SO(4). The extraction parameters are studied, and the behaviour of some other ions is reported. The method is used for ore analysis.

  2. Boiling heat transfer in dilute emulsions

    CERN Document Server

    Roesle, Matthew Lind


    Boiling Heat Transfer in Dilute Emulsions synthesizes recent advances and established understanding on the subject of boiling in dilute emulsions. Experimental results from various sources are collected and analyzed, including contemporary experiments that correlate visualization with heat transfer data. Published models of boiling heat transfer in dilute emulsions, and their implementation, are described and assessed against experimental data.

  3. Determination of cocaine in postmortem human liver exposed to overdose. Application of an innovative and efficient extraction/clean up procedure and gas chromatography-mass spectrometry analysis. (United States)

    Magalhães, Elisângela Jaqueline; Ribeiro de Queiroz, Maria Eliana Lopes; Penido, Marcus Luiz de Oliveira; Paiva, Marco Antônio Ribeiro; Teodoro, Janaína Aparecida Reis; Augusti, Rodinei; Nascentes, Clésia Cristina


    A simple and efficient method was developed for the determination of cocaine in post-mortem samples of human liver via solid-liquid extraction with low temperature partitioning (SLE-LTP) and analysis by gas chromatography coupled to mass spectrometry (GC-MS). The extraction procedure was optimized by evaluating the influence of the following variables: pH of the extract, volume and composition of the extractor solvent, addition of a sorbent material (PSA: primary-secondary amine) and NaCl to clean up and increase the ionic strength of the extract. A bovine liver sample that was free of cocaine was used as a blank for the optimization of the SLE-LTP extraction procedure. The highest recovery was obtained when crushed bovine liver (2g) was treated with 2mL of ultrapure water plus 8mL of acetonitrile at physiological pH (7.4). The results also indicated no need for using PSA and NaCl. The complete analytical procedure was validated for the following figures of merit: selectivity, lower limit of quantification (LLOQ), calibration curve, recovery, precision and accuracy (for within-run and between-run experiments), matrix effect, dilution integrity and stability. The within-run and between-run precision (at four levels) varied from 2.1% to 9.4% and from 4.0% to 17.0%, respectively. A maximum deviation of 11.62% for the within-run and between-run accuracies in relation to the nominal concentrations was observed. Moreover, the LLOQ value for cocaine was 50.0ngg(-1) whereas no significant effects were noticed in the assays of dilution integrity and stability. To assess its overall performance, the optimized method was applied to the analysis of eight human liver samples collected from individuals who died due to the abusive consumption of cocaine. Due to the existence of a significant matrix effect, a blank human liver was used to construct a matrix-matched analytical curve. The concentrations of cocaine found in these samples ranged from 333.5 to 5969ngg(-1). Copyright

  4. Comparison of DNA extraction methods for meat analysis. (United States)

    Yalçınkaya, Burhanettin; Yumbul, Eylem; Mozioğlu, Erkan; Akgoz, Muslum


    Preventing adulteration of meat and meat products with less desirable or objectionable meat species is important not only for economical, religious and health reasons, but also, it is important for fair trade practices, therefore, several methods for identification of meat and meat products have been developed. In the present study, ten different DNA extraction methods, including Tris-EDTA Method, a modified Cetyltrimethylammonium Bromide (CTAB) Method, Alkaline Method, Urea Method, Salt Method, Guanidinium Isothiocyanate (GuSCN) Method, Wizard Method, Qiagen Method, Zymogen Method and Genespin Method were examined to determine their relative effectiveness for extracting DNA from meat samples. The results show that the salt method is easy to perform, inexpensive and environmentally friendly. Additionally, it has the highest yield among all the isolation methods tested. We suggest this method as an alternative method for DNA isolation from meat and meat products. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Microprobe analysis of brine shrimp grown on meteorite extracts

    Energy Technology Data Exchange (ETDEWEB)

    Kennedy, J. [National Isotope Centre, GNS Science, 30 Gracefield Road, Lower Hutt (New Zealand)]. E-mail:; Mautner, M.N. [Soil, Plant and Ecological Sciences Division, Lincoln University (New Zealand) and Department of Chemistry, University of Canterbury, Christchurch 8001 (New Zealand)]. E-mail:; Barry, B. [National Isotope Centre, GNS Science, 30 Gracefield Road, Lower Hutt (New Zealand); Markwitz, A. [National Isotope Centre, GNS Science, 30 Gracefield Road, Lower Hutt (New Zealand)


    Nuclear microprobe methods have been used to investigate the uptake and distribution of various elements by brine shrimps and their unhatched eggs when grown in extracts of the Murchison and Allende carbonaceous meteorites, which were selected as model space resources. Measurements were carried out using a focussed 2 MeV proton beam raster scanned over the samples in order to obtain the average elemental concentrations. Line scans across the egg and shrimp samples show uptake of elements such as Mg, Ni, S and P which are present in the meteorites. The results confirmed that carbonaceous chondrite materials can provide nutrients, including high levels of the essential nutrient phosphate. The concentrations of these elements varied significantly between shrimp and eggs grown in extracts of the two meteorite types, which can help in identifying optimal growth media. Our results illustrate that nuclear microprobe techniques can determine elemental concentrations in organisms exposed to meteorite derived media and thus help in identifying useful future resources.

  6. Model analysis of mechanisms controlling pneumatic soil vapor extraction

    DEFF Research Database (Denmark)

    Høier, Camilla Kruse; Sonnenborg, Torben Obel; Jensen, Karsten Høgh;


    The efficiency of traditional soil venting or soil vapor extraction (SVE) highly depends on the architecture of the subsurface because imposed advective air flow tends to bypass low-permeable contaminated areas. Pneumatic SVE is a technique developed to enhance remediation efficiency of heterogen...... level the pneumatic venting technology is superior to the traditional technique, and that the method is particularly efficient in cases where large permeability contrasts exist between soil units in the subsurface.......The efficiency of traditional soil venting or soil vapor extraction (SVE) highly depends on the architecture of the subsurface because imposed advective air flow tends to bypass low-permeable contaminated areas. Pneumatic SVE is a technique developed to enhance remediation efficiency...... of heterogeneous soils by enforcing large fluctuating pressure fronts through the contaminated area. Laboratory experiments have suggested that pneumatic SVE considerably improves the recovery rate from low-permeable units. We have analyzed the experimental results using a numerical code and quantified...

  7. Gas chromatography-mass spectroscopy analysis of bioactive petalostigma extracts: Toxicity, antibacterial and antiviral activities

    Directory of Open Access Journals (Sweden)

    F R Kalt


    Full Text Available Background: Petalostigma pubescens and Petalostigma triloculare were common components of pharmacopeia′s of multiple Australian Aboriginal tribal groupings which traditionally inhabited the areas in which they grow. Among these groups, they had a myriad of medicinal uses in treating a wide variety of bacterial, fungal and viral infections. This study was undertaken to test P. pubescens and P. triloculare leaf and fruit extracts for the ability to inhibit bacterial and viral growth and thus validate Australian Aboriginal usage of these plants in treating bacterial and fungal diseases. Materials and Methods: P. pubescens, and P. triloculare leaves and fruit were extracted and tested for antimicrobial, antiviral activity and toxicity. The bioactive extracts were further examined by RP-HPLC and GC-MS to identify the component compounds. Results: The methanol, water and ethyl acetate leaf and fruit extracts of displayed potent antibacterial activity. The methanol and ethyl acetate extracts displayed the broadest specificity, inhibiting the growth of 10 of the 14 bacteria tested (71% for the leaf extract and 9 of the 14 bacteria tested (64% for the fruit extracts. The water extracts also had broad spectrum antibacterial activity, inhibiting the growth of 8 (57% and 7 (50% of the 14 bacteria tested, respectively. All antibacterial extracts were approximately equally effective against Gram-positive and Gram-negative bacteria, inhibiting the growth of 50-75% of the bacteria tested. The methanol, water and ethyl acetate extracts also displayed antiviral activity in the MS2 plaque reduction assay. The methanol and water extracts inhibited 26.6-49.0% and 85.4-97.2% of MS2 plaque formation, respectively, with the fruit extracts being more potent inhibitors. All ethyl acetate extracts inhibited 100% of MS2 plaque formation. All extracts were also non-toxic or of low toxicity. Analysis of these extracts by RP-HPLC showed that the P. triloculare ethyl acetate

  8. A Dilute-and-Shoot LC-MS Method for Quantitating Opioids in Oral Fluid. (United States)

    Enders, Jeffrey R; McIntire, Gregory L


    Opioid testing represents a dominant share of the market in pain management clinical testing facilities. Testing of this drug class in oral fluid (OF) has begun to rise in popularity. OF analysis has traditionally required extensive clean-up protocols and sample concentration, which can be avoided. This work highlights the use of a fast, 'dilute-and-shoot' method that performs no considerable sample manipulation. A quantitative method for the determination of eight common opioids and associated metabolites (codeine, morphine, hydrocodone, hydromorphone, norhydrocodone, oxycodone, noroxycodone and oxymorphone) in OF is described herein. OF sample is diluted 10-fold in methanol/water and then analyzed using an Agilent chromatographic stack coupled with an AB SCIEX 4500. The method has a 2.2-min LC gradient and a cycle time of 2.9 min. In contrast to most published methods of this particular type, this method uses no sample clean-up or concentration and has a considerably faster LC gradient, making it ideal for very high-throughput laboratories. Importantly, the method requires only 100 μL of sample and is diluted 10-fold prior to injection to help with instrument viability. Baseline separation of all isobaric opioids listed above was achieved on a phenyl-hexyl column. The validated calibration range for this method is 2.5-1,000 ng/mL. This 'dilute-and-shoot' method removes the unnecessary, costly and time-consuming extraction steps found in traditional methods and still surpasses all analytical requirements. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email:

  9. Cluster Analysis of Customer Reviews Extracted from Web Pages

    Directory of Open Access Journals (Sweden)

    S. Shivashankar


    Full Text Available As e-commerce is gaining popularity day by day, the web has become an excellent source for gathering customer reviews / opinions by the market researchers. The number of customer reviews that a product receives is growing at very fast rate (It could be in hundreds or thousands. Customer reviews posted on the websites vary greatly in quality. The potential customer has to read necessarily all the reviews irrespective of their quality to make a decision on whether to purchase the product or not. In this paper, we make an attempt to assess are view based on its quality, to help the customer make a proper buying decision. The quality of customer review is assessed as most significant, more significant, significant and insignificant.A novel and effective web mining technique is proposed for assessing a customer review of a particular product based on the feature clustering techniques, namely, k-means method and fuzzy c-means method. This is performed in three steps : (1Identify review regions and extract reviews from it, (2 Extract and cluster the features of reviews by a clustering technique and then assign weights to the features belonging to each of the clusters (groups and (3 Assess the review by considering the feature weights and group belongingness. The k-means and fuzzy c-means clustering techniques are implemented and tested on customer reviews extracted from web pages. Performance of these techniques are analyzed.


    Directory of Open Access Journals (Sweden)

    J Živković


    Full Text Available Proanthocyanidins, also known as condensed tannins are widespread in woody plants, but are also found in certain forages. Castanea sativa Mill. are exploited for various purposes, but a little is known about potential of this species and possible application in diet and therapy. The parts of chestnut such as: seed, peeled seed, brown seed shell, red internal seed shell, leaves, catkin, spiny bur, as well as the new and old chestnut bark were extracted with 50% ethanol as an extragents. Contents of total phenolics and total flavonoids were measured by application of the standard colorimetric assay. The total condensed tannins content estimated was highest in red internal seed shell 15.29%CE (vanillin assay and 3.12%CT (acid butanol assay. Also high content of total phenolic compounds and condensed tannins had extracts of catkin, brown seed shell of chestnut and new chestnut bark. Extracts of C. sativa Mill. can be a potential resource of natural tannins with possible application in diet and therapy.

  11. Analysis of entropy extraction efficiencies in random number generation systems (United States)

    Wang, Chao; Wang, Shuang; Chen, Wei; Yin, Zhen-Qiang; Han, Zheng-Fu


    Random numbers (RNs) have applications in many areas: lottery games, gambling, computer simulation, and, most importantly, cryptography [N. Gisin et al., Rev. Mod. Phys. 74 (2002) 145]. In cryptography theory, the theoretical security of the system calls for high quality RNs. Therefore, developing methods for producing unpredictable RNs with adequate speed is an attractive topic. Early on, despite the lack of theoretical support, pseudo RNs generated by algorithmic methods performed well and satisfied reasonable statistical requirements. However, as implemented, those pseudorandom sequences were completely determined by mathematical formulas and initial seeds, which cannot introduce extra entropy or information. In these cases, “random” bits are generated that are not at all random. Physical random number generators (RNGs), which, in contrast to algorithmic methods, are based on unpredictable physical random phenomena, have attracted considerable research interest. However, the way that we extract random bits from those physical entropy sources has a large influence on the efficiency and performance of the system. In this manuscript, we will review and discuss several randomness extraction schemes that are based on radiation or photon arrival times. We analyze the robustness, post-processing requirements and, in particular, the extraction efficiency of those methods to aid in the construction of efficient, compact and robust physical RNG systems.

  12. The complete targeted profile of the organic acid intermediates of the citric acid cycle using a single stable isotope dilution analysis, sodium borodeuteride reduction and selected ion monitoring GC/MS. (United States)

    Mamer, Orval; Gravel, Simon-Pierre; Choinière, Luc; Chénard, Valérie; St-Pierre, Julie; Avizonis, Daina


    The quantitative profiling of the organic acid intermediates of the citric acid cycle (CAC) presents a challenge due to the lack of commercially available internal standards for all of the organic acid intermediates. We developed an analytical method that enables the quantitation of all the organic acids in the CAC in a single stable isotope dilution GC/MS analysis with deuterium-labeled analogs used as internal standards. The unstable α-keto acids are rapidly reduced with sodium borodeuteride to the corresponding stable α-deutero-α-hydroxy acids and these, along with their unlabeled analogs and other CAC organic acid intermediates, are converted to their tert-butyldimethylsilyl derivatives. Selected ion monitoring is employed with electron ionization. We validated this method by treating an untransformed mouse mammary epithelial cell line with well-known mitochondrial toxins affecting the electron transport chain and ATP synthase, which resulted in profound perturbations of the concentration of CAC intermediates.

  13. The GC/MS Analysis of Volatile Components Extracted by Different Methods from Exocarpium Citri Grandis

    Directory of Open Access Journals (Sweden)

    Zhisheng Xie


    Full Text Available Volatile components from Exocarpium Citri Grandis (ECG were, respectively, extracted by three methods, that is, steam distillation (SD, headspace solid-phase microextraction (HS-SPME, and solvent extraction (SE. A total of 81 compounds were identified by gas chromatography-mass spectrometry including 77 (SD, 56 (HS-SPME, and 48 (SE compounds, respectively. Despite of the extraction method, terpenes (39.98~57.81% were the main volatile components of ECG, mainly germacrene-D, limonene, 2,6,8,10,14-hexadecapentaene, 2,6,11,15-tetramethyl-, (E,E,E-, and trans-caryophyllene. Comparison was made among the three methods in terms of extraction profile and property. SD relatively gave an entire profile of volatile in ECG by long-time extraction; SE enabled the analysis of low volatility and high molecular weight compounds but lost some volatiles components; HS-SPME generated satisfactory extraction efficiency and gave similar results to those of SD at analytical level when consuming less sample amount, shorter extraction time, and simpler procedure. Although SD and SE were treated as traditionally preparative extractive techniques for volatiles in both small batches and large scale, HS-SPME coupled with GC/MS could be useful and appropriative for the rapid extraction and qualitative analysis of volatile components from medicinal plants at analytical level.

  14. Comparison of different extraction solutions for the analysis of allergens in hen's egg. (United States)

    Hildebrandt, S; Steinhart, H; Paschke, A


    An important requirement for the correct procedure of allergen analysis in hen's egg is to obtain complete and unaltered protein extracts. Besides the aim of a quantitative extraction of the allergens from the matrix, it is equally important not to alter their allergenic potential during the extraction process. This paper describes and compares six extraction solutions for the analysis of whole-egg proteins and allergens. These requirements were examined via protein determination according to Bradford [Bradford, M. M. (1976). Rapid and sensitive method for quantitation of microgram quantities of protein utilizing principle of protein-dye binding. Analytical Biochemistry, 72, 248-254] and Kjeldahl [Meyer, A. H. (2006). Lebensmittelrecht, Verlag C.H. Beck München, Stand: 1. February 2006, § 64, Lebensmittel- und Futtermittelgesetzbuch, Amtliche Sammlung von Untersuchungsmethoden, Nr. L 06.00-7] as well as the EAST-inhibition method. It could be demonstrated that the extraction with a urea solution (8M) led to significant interferences during the protein determination, and substantially reduced the allergenic potential of egg proteins. With all other extraction solutions adequate protein contents could be extracted. The highest protein content was achieved by the extraction with phosphate buffered saline followed by a Tween 20 solution, physiological saline, water, and acetate buffer. The results show that none of these extracts - except for the urea solution (8M) - was altered in its' allergenic potential.


    Directory of Open Access Journals (Sweden)

    Parixit Bhandurge


    Full Text Available Fenugreek (Trigonella foenum-graecumL. Leguminosae is widely used in Indian Ayurvedic medicine for the treatment of diabetes mellitus. Antihyperglycaemic effect of the two different doses (200 and 400 mg/kg of the fenugreek extract was evaluated in this study. Blood glucose, liver profile, renal profile and total lipid levels were determined in alloxan induced diabetic rats after oral administration of a fenugreek extract. A comparable hypoglycemic effect was evidenced from the data obtained after 7 and 21 days of oral administration of the extract. The extract lowered the total cholesterol and serum triglycerides. Histopathological analysis of pancreas showed normal acini, and normal cellular in the islets of langerhans in the pancreas of normal control and Extensive damage to islets of langerhans and reduced dimensions of islets in alloxan induced diabetes. Restoration of islets of langerhans seen in diabetic rats treated with fenugreek extract. The results of this study clearly shows the hypoglycaemic activity of the extract

  16. Background Extraction Method Based on Block Histogram Analysis for Video Image

    Institute of Scientific and Technical Information of China (English)

    Li Hua; Peng Qiang


    A novel method of histogram analysis for background extraction in video image is proposed, which is derived from the pixelbased histogram analysis. Not only the statistical property of pixels between temporal frames, but also the correlation of local pixels in a single frame is exploited in this method. When carrying out histogram analysis for background extraction, the proposed method is not based on a single pixel but on a 2×2 block that has much less computational quantities and can extract a sound background image from video sequence simultaneously. A comparative experiment between the proposed method and the pixel-based histogram analysis shows that the proposed method has a faster speed in background extraction and the obtained background image is better in quantity.

  17. Application of supercritical fluid carbon dioxide to the extraction and analysis of lipids. (United States)

    Lee, Jae Won; Fukusaki, Eiichiro; Bamba, Takeshi


    Supercritical carbon dioxide (SCCO(2)) is an ecofriendly supercritical fluid that is chemically inert, nontoxic, noninflammable and nonpolluting. As a green material, SCCO(2) has desirable properties such as high density, low viscosity and high diffusivity that make it suitable for use as a solvent in supercritical fluid extraction, an effective and environment-friendly analytical method, and as a mobile phase for supercritical fluid chromatography, which facilitates high-throughput, high-resolution analysis. Furthermore, the low polarity of SCCO(2) is suitable for the extraction and analysis of hydrophobic compounds. The growing concern surrounding environmental pollution has triggered the development of green analysis methods based on the use of SCCO(2) in various laboratories and industries. SCCO(2) is becoming an effective alternative to conventional organic solvents. In this review, the usefulness of SCCO(2) in supercritical fluid extraction and supercritical fluid chromatography for the extraction and analysis of lipids is described.

  18. Performance analysis of a hybrid fingerprint extracted from optical coherence tomography fingertip scans

    CSIR Research Space (South Africa)

    Darlow, Luke N


    Full Text Available International Conference on Biometrics (ICB), 13-16 June 2016, Halmstad, Sweden Performance analysis of a hybrid fingerprint extracted from optical coherence tomography fingertip scans Darlow LN Connan J Singh A ABSTRACT: The Hybrid fingerprint is a...

  19. Turbulence in dilute polymer solutions (United States)

    Liberzon, A.; Guala, M.; Lüthi, B.; Kinzelbach, W.; Tsinober, A.


    The work reported below is a comparative study of the properties of turbulence with weak mean flow in a Newtonian fluid and in a dilute polymer solution with an emphasis on the small scale phenomena. The main tool used is a three-dimensional particle tracking system allowing to measure and follow in a Lagrangian manner the field of velocities, as well as velocity derivatives, and thus vorticity, strain, and a variety of related and dynamically significant quantities. The comparison of data from the two flows allows to directly observe the influence of polymers on these quantities as well as the evolution of material elements in the presence of polymers.

  20. Optimal Fixation Conditions and DNA Extraction Methods for MLPA Analysis on FFPE Tissue-Derived DNA. (United States)

    Atanesyan, Lilit; Steenkamer, Maryvonne J; Horstman, Anja; Moelans, Cathy B; Schouten, Jan P; Savola, Suvi P


    Molecular genetic analysis of formalin-fixed, paraffin-embedded (FFPE) tissues is of great importance both for research and diagnostics. Multiplex ligation-dependent probe amplification (MLPA) is a widely used technique for gene copy number determination, and it has been successfully used for FFPE tissue-extracted DNA analysis. However, there have been no studies addressing the effect of tissue fixation procedures and DNA extraction methods on MLPA. This study therefore focuses on selecting optimal preanalytic conditions such as FFPE tissue preparation conditions and DNA extraction methods. Healthy tissues were fixed in buffered or nonbuffered formalin for 1 hour, 12 to 24 hours, or 48 to 60 hours at 4 °C or at room temperature. DNA extracted from differently fixed and subsequently paraffin-embedded tissues was used for MLPA. Four commercial DNA extraction kits and one in-house method were compared. Tissues fixed for 12 to 24 hours in buffered formalin at room temperature produced DNA with the most optimal quality for MLPA. The in-house FFPE DNA extraction method was shown to perform as efficient as or even superior to other methods in terms of suitability for MLPA, time and cost-efficiency, and ease of performance. FFPE-extracted DNA is well suitable for MLPA analysis, given that optimal tissue fixation and DNA extraction methods are chosen.

  1. Hexafluoroisopropanol-induced catanionic-surfactants-based coacervate extraction for analysis of lysozyme. (United States)

    Xu, Jia; Niu, Manli; Xiao, Yuxiu


    A coacervate extraction method, based on hexafluoroisopropanol (HFIP)-induced catanionic surfactants and coupled with a back-extraction procedure, was developed for separation and purification of proteins, using sodium dodecyl sulfate (SDS) and dodecyltrimethyl ammonium bromide (DTAB) as representative catanionic surfactants and lysozyme as a model protein. After the coacervate extraction and back extraction, the obtained lysozyme solutions were examined in terms of quantitative analysis by capillary electrophoresis, bacteriolytic activity, and circular dichroism (CD). The effects of several parameters including back-extraction solvent, HFIP content, total surfactant concentration, and SDS/DTAB molar ratio were investigated in detail on the extraction efficiency and activity of lysozyme. Under the optimized extraction conditions (66 mM KH2PO4 buffer with pH 6.2 as back-extraction solvent, SDS/DTAB molar ratio = 1:1 mol/mol, total surfactant concentration = 30 mM, HIFP concentration = 8 % v/v), the extraction recovery was 89.8 % (±4.7, n = 3), limit of detection was 2.2 (±0.3, n = 3) μg mL(-1), and meanwhile nearly 65 % of native lysozyme activity was retained. In addition, the activity and CD assays showed that SDS/DTAB molar ratio had a significant influence on the activity and structure of lysozyme after extraction. The DTAB-rich extraction systems, in which the DTAB mole fraction was equal to or larger than 70 %, could keep the activity and structure of lysozyme almost in the native state. Graphical Abstract Procedure of HFIP-induced SDS/DTAB coacervate extraction and back extraction of lysozyme.

  2. Comprehensive automation of the solid phase extraction gas chromatographic mass spectrometric analysis (SPE-GC/MS) of opioids, cocaine, and metabolites from serum and other matrices. (United States)

    Lerch, Oliver; Temme, Oliver; Daldrup, Thomas


    The analysis of opioids, cocaine, and metabolites from blood serum is a routine task in forensic laboratories. Commonly, the employed methods include many manual or partly automated steps like protein precipitation, dilution, solid phase extraction, evaporation, and derivatization preceding a gas chromatography (GC)/mass spectrometry (MS) or liquid chromatography (LC)/MS analysis. In this study, a comprehensively automated method was developed from a validated, partly automated routine method. This was possible by replicating method parameters on the automated system. Only marginal optimization of parameters was necessary. The automation relying on an x-y-z robot after manual protein precipitation includes the solid phase extraction, evaporation of the eluate, derivatization (silylation with N-methyl-N-trimethylsilyltrifluoroacetamide, MSTFA), and injection into a GC/MS. A quantitative analysis of almost 170 authentic serum samples and more than 50 authentic samples of other matrices like urine, different tissues, and heart blood on cocaine, benzoylecgonine, methadone, morphine, codeine, 6-monoacetylmorphine, dihydrocodeine, and 7-aminoflunitrazepam was conducted with both methods proving that the analytical results are equivalent even near the limits of quantification (low ng/ml range). To our best knowledge, this application is the first one reported in the literature employing this sample preparation system.

  3. Feature Extraction and Analysis of Breast Cancer Specimen (United States)

    Bhattacharyya, Debnath; Robles, Rosslin John; Kim, Tai-Hoon; Bandyopadhyay, Samir Kumar

    In this paper, we propose a method to identify abnormal growth of cells in breast tissue and suggest further pathological test, if necessary. We compare normal breast tissue with malignant invasive breast tissue by a series of image processing steps. Normal ductal epithelial cells and ductal / lobular invasive carcinogenic cells also consider for comparison here in this paper. In fact, features of cancerous breast tissue (invasive) are extracted and analyses with normal breast tissue. We also suggest the breast cancer recognition technique through image processing and prevention by controlling p53 gene mutation to some greater extent.

  4. 稻草秸秆超低酸水解及水解产物分析%Hydrolysis of Rice Straw with Extremely Dilute Acid and Products Analysis

    Institute of Scientific and Technical Information of China (English)

    王为国; 李自豪; 覃远航; 吕仁亮; 张俊峰; 王存文


    The hydrolysis of rice straw with extremely dilute sulfuric acid(0.05%(w)) was conducted.It was found that the optimal solid content and stirring speed for the rice straw hydrolysis were 0.050 0 g/mL and 700 r/min,respectively.The change of the hydrolysis with time was investigated in the temperature range of 160-210 ℃.The results indicated that,in the hydrolysis,there was a single-peak of reducing sugar content at 160 ℃,in the temperature range of 170-200 ℃there was a double-peak,and a single-peak reappeared at 210 ℃.The reason was that the reducing sugar concentration from the hydrolysis of hemicellulose and cellulose showed two peaks,and the peaks superimposed or separated as the hydrolysis temperature changed.The hydrolysis products and solid residues were characterized by means of FTIR and HPLC.The results showed that,most of hemicellulose hydrolyzed and disappeared,the structure of the lignin was destroyed to a certain extent,the polymerization degree of the cellulose decreased greatly but its crystallinity was still high.The main hydrolysis products were cellotriose,cellobiose,glucose,xylose,methylglyoxal and some unknown compounds.%用0.05%(w)的稀硫酸对湖北省稻草秸秆进行水解,考察了混合原料中固体含量和搅拌转速对稻草秸秆水解的影响.实验结果表明,最佳秸秆颗粒的质量浓度为0.050 0 g/mL,最佳转速为700 r/min.研究了稻草秸秆在160~ 210℃内的水解趋势.研究结果表明,160℃时,稻草秸秆水解得到的还原糖含量随水解的进行呈单峰趋势;在170~ 200℃时呈双峰趋势;当温度达到210℃时又呈现单峰趋势,这与稻草秸秆中纤维素和半纤维素水解得到的两个还原糖峰随水解的进行呈现叠加和分离有关.表征固体残渣并分析水解产物组成的结果显示,水解后半纤维素大部分水解,木质素的结构在一定程度上被破坏,纤维素的聚合度急剧降低但结晶度仍较高;水解产物主要为

  5. Analysis of Key Odorants in Roasted Green Tea (United States)

    Mizukami, Yuzo; Sawai, Yusuke; Yamaguchi, Yuichi

    This research aims to identify key odorants in roasted green tea. The aroma extract dilution analysis revealed 25 odor-active peaks with the flavor dilution factors of ≥ 16. We identified 2-ethyl-3,5-dimethylpyrazine as the most important odorant in roasted green tea with the highest flavor dilution factor of 4096. In addition, tetramethylpyrazine, 2,3-diethyl-5- methylpyrazine were also detected as potent odorants with the high flavor dilution factors. These three alkylpyrazines would be key contributors to aroma of roasted green tea.

  6. Efficiency dilution: long-term exergy conversion trends in Japan. (United States)

    Williams, Eric; Warr, Benjamin; Ayres, Robert U


    This analysis characterizes century-scale trends in exergy efficiency in Japan. Exergy efficiency captures the degree to which energy inputs (such as coal) are converted into useful work (such as electricity or power to move a vehicle). This approach enables the estimation of net efficiencies which aggregate different technologies. Sectors specifically analyzed are electricity generation, transport, steel production, and residential space heating. One result is that the aggregate exergy efficiency of the Japanese economy declined slightly over the last half of the 20th century, reaching a high of around 38% in the late 1970s and falling to around 33% by 1998. The explanation for this is that while individual technologies improved dramatically over the century, less exergy-efficient ones were progressively adopted, yielding a net stabilization or decline. In the electricity sector, for instance, adoption of hydropower was followed by fossil-fired plants and then by nuclear power, each technology being successively less efficient from an exergy perspective. The underlying dynamic of this trend is analogous to declining ore grades in the mining sector. Increasing demand for exergy services requires expended utilization of resources from which it is more difficult to extract utility (e.g., falling water versus coal). We term this phenomenon efficiency dilution.

  7. Simple and sensitive analysis of histamine and tyramine in Japanese soy sauces and their intermediates using the stable isotope dilution HILIC-MS/MS method. (United States)

    Todoroki, Kenichiro; Ishii, Yasuhiro; Miyauchi, Chiemi; Kitagawa, Sachiyo; Min, Jun Zhe; Inoue, Koichi; Yamanaka, Tomoyuki; Suzuki, Kuniaki; Yoshikawa, Yuko; Ohashi, Norio; Toyo'oka, Toshimasa


    We established a simple, sensitive, and reproducible method to analyze the histamine and tyramine levels in Japanese soy sauce and its mash (called moromi) using hydrophilic interaction liquid chromatography with tandem mass spectrometry (HILIC-MS/MS). Histamine and tyramine quantification was performed using their stable isotopes for electrospray ionization-tandem mass spectrometry in the selected reaction monitoring mode. The sample pretreatment process was a simple, one-step liquid-liquid extraction. HILIC separation was performed with a gradient elution of aqueous ammonium formate and acetonitrile. Because of validation tests, the linearity, the accuracies, and precisions were sufficient. The limit of detection and the limit of quantification were 0.09 and 0.29 ppm for histamine and 0.13 and 0.42 ppm for tyramine, respectively. We successfully applied this method to histamine and tyramine determination in four kinds of commercial Japanese soy sauces and also in moromi samples during soy sauce production.

  8. Dilute Acid and Autohydrolysis Pretreatment (United States)

    Yang, Bin; Wyman, Charles E.

    Exposure of cellulosic biomass to temperatures of about 120-210°C can remove most of the hemicellulose and produce cellulose-rich solids from which high glucose yields are possible with cellulase enzymes. Furthermore, the use of dilute sulfuric acid in this pretreatment operation can increase recovery of hemicellulose sugars substantially to about 85-95% of the maximum possible versus only about 65% if no acid is employed. The use of small-diameter tubes makes it possible to employ high solids concentrations similar to those preferred for commercial operations, with rapid heat-up, good temperature control, and accurate closure of material balances. Mixed reactors can be employed to pretreat larger amounts of biomass than possible in such small-diameter tubes, but solids concentrations are limited to about 15% or less to provide uniform temperatures. Pretreatment of large amounts of biomass at high solids concentrations is best carried out using direct steam injection and rapid pressure release, but closure of material balances in such “steam gun” devices is more difficult. Although flow of water alone or containing dilute acid is not practical commercially, such flow-through configurations provide valuable insight into biomass deconstruction kinetics not possible in the batch tubes, mixed reactors, or steam gun systems.

  9. Guideline on Isotope Dilution Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Gaffney, Amy [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)


    Isotope dilution mass spectrometry is used to determine the concentration of an element of interest in a bulk sample. It is a destructive analysis technique that is applicable to a wide range of analytes and bulk sample types. With this method, a known amount of a rare isotope, or ‘spike’, of the element of interest is added to a known amount of sample. The element of interest is chemically purified from the bulk sample, the isotope ratio of the spiked sample is measured by mass spectrometry, and the concentration of the element of interest is calculated from this result. This method is widely used, although a mass spectrometer required for this analysis may be fairly expensive.

  10. Dilute Potts model in two dimensions. (United States)

    Qian, Xiaofeng; Deng, Youjin; Blöte, Henk W J


    We study the two-dimensional dilute q-state Potts model by means of transfer-matrix and Monte Carlo methods. Using the random-cluster representation, we include noninteger values of q. We locate phase transitions in the three-dimensional parameter space of q, the Potts coupling K>0, and the chemical potential of the vacancies. The critical plane is found to contain a line of fixed points that divides into a critical branch and a tricritical one, just as predicted by the renormalization scenario formulated by Nienhuis et al for the dilute Potts model. The universal properties along the line of fixed points agree with the theoretical predictions. We also determine the density of the vacancies along these branches. For q=2-squareroot of 2 we obtain the phase diagram in a three-dimensional parameter space that also includes a coupling V> or = 0 between the vacancies. For q=2, the latter space contains the Blume-Capel model as a special case. We include a determination of the tricritical point of this model, as well as an analysis of percolation clusters constructed on tricritical Potts configurations for noninteger q. This percolation study is based on Monte Carlo algorithms that include local updates flipping between Potts sites and vacancies. The bond updates are performed locally for and by means of a cluster algorithm for q>1. The updates for q>1 use a number of operations per site independent of the system size.

  11. Vacuum Permeator Analysis for Extraction of Tritium from DCLL Blankets

    Energy Technology Data Exchange (ETDEWEB)

    Humrickhouse, Paul Weston [Idaho National Laboratory; Merrill, Brad Johnson [Idaho National Laboratory


    It is envisioned that tritium will be extracted from DCLL blankets using a vacuum permeator. We derive here an analytical solution for the extraction efficiency of a permeator tube, which is a function of only two dimensionless numbers: one that indicates whether radial transport is limited in the PbLi or in the solid membrane, and another that is the ratio of axial and radial transport times in the PbLi. The permeator efficiency is maximized by decreasing the velocity and tube diameter, and increasing the tube length. This is true regardless of the mass transport correlation used; we review several here and find that they differ little, and the choice of correlation is not a source of significant uncertainty here. The PbLi solubility, on the other hand, is a large source of uncertainty, and we identify upper and lower bounds from the literature data. Under the most optimistic assumptions, we find that a ferritic steel permeator operating at 550 °C will need to be at least an order of magnitude larger in volume than previous conceptual designs using niobium and operating at higher temperatures.

  12. Extraction, Purification, and NMR Analysis of Terpenes from Brown Algae. (United States)

    Gaysinski, Marc; Ortalo-Magné, Annick; Thomas, Olivier P; Culioli, Gérald


    Algal terpenes constitute a wide and well-documented group of marine natural products with structures differing from their terrestrial plant biosynthetic analogues. Amongst macroalgae, brown seaweeds are considered as one of the richest source of biologically and ecologically relevant terpenoids. These metabolites, mostly encountered in algae of the class Phaeophyceae, are mainly diterpenes and meroditerpenes (metabolites of mixed biogenesis characterized by a toluquinol or a toluquinone nucleus linked to a diterpene moiety).In this chapter, we describe analytical processes commonly employed for the isolation and structural characterization of the main terpenoid constituents obtained from organic extracts of brown algae. The successive steps include (1) extraction of lipidic content from algal samples; (2) purification of terpenes by column chromatography and semi-preparative high-performance liquid chromatography; and (3) structure elucidation of the isolated terpenes by means of 1D and 2D nuclear magnetic resonance (NMR). More precisely, we propose a representative methodology which allows the isolation and structural determination of the monocyclic meroditerpene methoxybifurcarenone (MBFC) from the Mediterranean brown alga Cystoseira amentacea var. stricta. This methodology has a large field of applications and can then be extended to terpenes isolated from other species of the family Sargassaceae.

  13. Extraction of soluble substances from organic solid municipal waste to increase methane production. (United States)

    Campuzano, Rosalinda; González-Martínez, Simón


    This work deals with the analysis of the methane production from Mexico City's urban organic wastes after separating soluble from suspended substances. Water was used to extract soluble substances under three different water to waste ratios and after three extraction procedures. Methane production was measured at 35 °C during 21 days using a commercial methane potential testing device. Results indicate that volatile solids extraction increases with dilution rate to a maximum of 40% at 20 °C and to 43% at 93 °C. The extracts methane production increases with the dilution rate as a result of enhanced dissolved solids extraction. The combined (extract and bagasse) methane production reached, in 6 days, 66% of the total methane produced in 21 days. The highest methane production rates were measured during the first six days.

  14. Optimization of an effective extraction procedure for the analysis of microcystins in soils and lake sediments

    Energy Technology Data Exchange (ETDEWEB)

    Chen Wei [State Key Laboratory of Freshwater Ecology and Biotechnology, Institute of Hydrobiology, Chinese Academy of Sciences, Wuhan 430072 (China); Graduate School of Chinese Academy of Sciences, Beijing 100049 (China); Li Lin [State Key Laboratory of Freshwater Ecology and Biotechnology, Institute of Hydrobiology, Chinese Academy of Sciences, Wuhan 430072 (China); Gan Nanqin [State Key Laboratory of Freshwater Ecology and Biotechnology, Institute of Hydrobiology, Chinese Academy of Sciences, Wuhan 430072 (China); Song Lirong [State Key Laboratory of Freshwater Ecology and Biotechnology, Institute of Hydrobiology, Chinese Academy of Sciences, Wuhan 430072 (China)]. E-mail:


    Microcystin analysis in sediments and soils is considered very difficult due to low recovery for extraction. This is the primary limiting factor for understanding the fate of toxins in the interface between water and sediment in both the aquatic ecosystem as well as in soils. In the present study, a wide range of extraction solvents were evaluated over a wide range of pH, extraction approaches and equilibration time to optimize an effective extraction procedure for the analysis of microcystins in soils and lake sediments. The number of extractions required and acids in extraction solutions were also studied. In this procedure, EDTA-sodium pyrophosphate solution was selected as an extraction solvent based on the adsorption mechanism study. The optimized procedure proved to be highly efficient and achieved over 90% recovery. Finally, the developed procedure was applied to field soil and sediment sample collected from Chinese lakes during bloom seasons and microcystins were determined in six of ten samples. - Efficiency of extraction of microcystins from soil and sediment was greatly increased.

  15. Antioxidant, DNA protective efficacy and HPLC analysis of Annona muricata (soursop) extracts. (United States)

    George, V Cijo; Kumar, D R Naveen; Suresh, P K; Kumar, R Ashok


    Annona muricata is a naturally occurring edible plant with wide array of therapeutic potentials. In India, it has a long history of traditional use in treating various ailments. The present investigation was carried out to characterize the phytochemicals present in the methanolic and aqueous leaf extracts of A. muricata, followed by validation of its radical scavenging and DNA protection activities. The extracts were also analyzed for its total phenolic contents and subjected to HPLC analysis to determine its active metabolites. The radical scavenging activities were premeditated by various complementary assays (DRSA, FRAP and HRSA). Further, its DNA protection efficacy against H2O2 induced toxicity was evaluated using pBR322 plasmid DNA. The results revealed that the extracts were highly rich in various phytochemicals including luteolin, homoorientin, tangeretin, quercetin, daidzein, epicatechin gallate, emodin and coumaric acid. Both the extracts showed significant (p < 0.05) radical scavenging activities, while methanolic extract demonstrated improved protection against H2O2-induced DNA damage when compared to aqueous extract. A strong positive correlation was observed for the estimated total phenolic contents and radical scavenging potentials of the extracts. Further HPLC analysis of the phyto-constituents of the extracts provides a sound scientific basis for compound isolation.

  16. Preliminary phytochemical screening, Antibacterial potential and GC-MS analysis of two medicinal plant extracts. (United States)

    Vijayaram, Seerangaraj; Kannan, Suruli; Saravanan, Konda Mani; Vasantharaj, Seerangaraj; Sathiyavimal, Selvam; P, Palanisamy Senthilkumar


    The presence study was aimed to catalyze the primary metabolites and their confirmation by using GC-MS analysis and antibacterial potential of leaf extract of two important medicinal plant viz., Eucalyptus and Azadirachta indica. The antibacterial potential of the methanol leaf extract of the studied species was tested against Escherichia coli, Pseudomonas aeruginosa, Klebsiellap neumoniae, Streptococcus pyogens, Staphylococcus aureus using by agar well diffusion method. The higher zone of inhibition (16mm) was observed against the bacterium Pseudomonas aeruginosa at 100μl concentration of methanol leaf extract. Preliminary phytochemical analysis of studied species shows that presence of phytochemical compounds like steroids, phenolic compounds and flavonoids. GC-MS analysis confirms the occurrence of 20 different compounds in the methanol leaf extract of the both studied species.

  17. Analysis of gamma irradiated pepper constituents, 3. The supercritical fluid extraction of pepper perfume

    Energy Technology Data Exchange (ETDEWEB)

    Takagi, Kazuko; Okuyama, Tsuneo; Yamauchi, Yoshio; Saito, Muneo.


    The extraction of pepper perfume by use of supercritical fluid extraction (SFE) was investigated. Carbon dioxide was used as supercritical mobile phase. SFE was achieved by follow conditions, temperature was 40deg C, pressure was 200 kgf/cm/sup 2/, 5 % methanol was added to mobile phase and the extraction time was 60 minutes. The extracted fraction by this method was yellow oily substance and was pepper perfume rich fraction, while the residue of extraction had not only perfume but also any pungency. And it seems that most part of pepper perfume was extracted by Supercritical fluid extraction. The perfume fraction was analyzed by two way method, that is, supercritical fluid chromatography (SFC) and reversed phase HPLC. SFC conditions were same as SFE. HPLC conditions were described as the first report. By both methods, about 7 peaks were detected. According to their analysis of this fraction, the main component was identified as piperine. On the chromatogram of reversed phase HPLC of extract, most peaks were eluted later than piperine. And it is thought that most perfume components have high hydrophobicity more than piperine. The change of perfume of pepper was able to be discussed based on the extraction by SFE.

  18. Phytochemical analysis of Myrtus communis plant: Conventional versus microwave assisted-extraction procedures. (United States)

    Bouaoudia-Madi, Nadia; Boulekbache-Makhlouf, Lila; Kadri, Nabil; Dahmoune, Farid; Remini, Hocine; Dairi, Sofiane; Oukhmanou-Bensidhoum, Sonia; Madani, Khodir


    Background Myrtle (Myrtus communis L) may constitute an interesting dietary source of health protective compounds. Microwave-assisted extraction (MAE) of total phenolic compounds (TPC) from myrtle leaf, stems, pericarp, and seeds was studied and the results were compared with those of the conventional method extraction (CME) in terms of extraction time. Methods Extraction yield/efficiency and antioxidant activity were measured using radical scavenging assay (DPPH•) and reducing power. Results The results show that the MAE was higher in terms of saving energy, extraction time (62 s) and extraction efficiency of bioactive compound compared to CME (2 h). Leaf presented the optimum content of total phenols (250 mg GAE.g-1 DW) and flavonoids (13.65 mg GAE.g-1 DW). However, the anthocyanin content was most important in pericarp extract (176.50±2.17 mg Cyd-3-glu g-1 DW). The antioxidant activity was important in all parts, mainly in leaves. The results indicated that appropriate microwave treatment could be an efficient process to phenolic compounds recovery and thus, better the antioxidant activity of myrtle extract. Conclusions Principal component analysis (PCA) applied to the experimental data shows that the distribution of the myrtle phenolic compounds depended on their plant part localization as well as the extraction method.

  19. Evaluation and validation of a single-dilution potency assay based upon serology of vaccines containing diphtheria toxoid: analysis for consistency in production and testing at the laboratory of the Control of Biological Products of the RIVM

    NARCIS (Netherlands)

    Akkermans AM; Hendriksen CFM; Marsman FR; de Jong WH; van de Donk HJM


    A single-dilution assay can be a valid procedure to demonstrate that a product exceeds the minimal requirement given for potency provided that consistency in production and testing has been proven. Information is presented justifying the use of a single dilution assay based upon quantitative respon

  20. Evaluation and validation of a single-dilution potency assay based upon serology of vaccines containing diphtheria toxoid: analysis for consistency in production and testing at the laboratory of the Control of Biological Products of the RIVM

    NARCIS (Netherlands)

    Akkermans AM; Hendriksen CFM; Marsman FR; de Jong WH; van de Donk HJM


    A single-dilution assay can be a valid procedure to demonstrate that a product exceeds the minimal requirement given for potency provided that consistency in production and testing has been proven. Information is presented justifying the use of a single dilution assay based upon quantitative respon

  1. A method to extract soil water for stable isotope analysis (United States)

    Revesz, K.; Woods, P.H.


    A method has been developed to extract soil water for determination of deuterium (D) and 18O content. The principle of this method is based on the observation that water and toluene form an azeotropic mixture at 84.1??C, but are completely immiscible at ambient temperature. In a specially designed distillation apparatus, the soil water is distilled at 84.1??C with toluene and is separated quantitatively in the collecting funnel at ambient temperature. Traces of toluene are removed and the sample can be analyzed by mass spectrometry. Kerosene may be substituted for toluene. The accuracy of this technique is ?? 2 and ?? 0.2???, respectively, for ??D and ??18O. Reduced accuracy is obtained at low water contents. ?? 1990.

  2. EKSTRAKSI DAN ANALISIS FITOSTEROL LEMBAGA GANDUM [Extraction and analysis of Phytosterol from wheat germ (Triticum sp.

    Directory of Open Access Journals (Sweden)

    Latifah K Darusman3


    Full Text Available Phytosterol may reduce the absorption of cholesterol, and used for preventing atherosclerosis. It is limited in soybean, but potentially abundant in wheat germ. Research on the utilization of wheat germ sterol had not been reported so far. Many aspects of germ sterol extraction from wheat germ and its characteristics were still unknown. In this research, the best extraction method, kinds and content of phytosterol from wheat germ were investigated.This research consisted of two steps: (1 extraction of phytosterol directly form whole germ and ground germ using hexane, and indirect extraction through germ oil using hexane and mixed solvent of hexane and ethanol, and direct extraction from ground germ using ethanol; (2 analysis of the type and content of phytosterol in the crude extract through the following steps: preparation of crude extract, fractionation, and analysis.Results showed that indirect extraction through germ oil was considered as the best method which yielded 1.37% of phytosterol. The highest yield was obtained when extracted using a mixed solvent of hexane – ethanol 82:18. However, the odor of ethanol and hexane (gasoline like odor was still detected. The solvent’s ratio of hexane to ethanol at 1:2 resulted better odor of the extract. Extraction of sterol using ethanol yielded 18.39% of sterol when the ratio of germ to ethanol at 1:10 (w/v was applied.Results of quantitative analysis on the main component of crude extract of wheat germ sterol showed that the total content of sterol extracted with mixed solvent was higher than those extracted with ethanol. The ratio of hexane to ethanol at 1:1 (v/v gave higher content of total sterol, stigmasterol and campesterol, whereas higher content of -sitosterol was produced at the solvent’s ratio of hexane to ethanol at 1:2 (v/v.

  3. Isolation and structural characterization of sugarcane bagasse lignin after dilute phosphoric acid plus steam explosion pretreatment and its effect on cellulose hydrolysis. (United States)

    Zeng, Jijiao; Tong, Zhaohui; Wang, Letian; Zhu, J Y; Ingram, Lonnie


    The structure of lignin after dilute phosphoric acid plus steam explosion pretreatment process of sugarcane bagasse in a pilot scale and the effect of the lignin extracted by ethanol on subsequent cellulose hydrolysis were investigated. The lignin structural changes caused by pretreatment were identified using advanced nondestructive techniques such as gel permeation chromatography (GPC), quantitative (13)C, and 2-D nuclear magnetic resonance (NMR). The structural analysis revealed that ethanol extractable lignin preserved basic lignin structure, but had relatively lower amount of β-O-4 linkages, syringyl/guaiacyl units ratio (S/G), p-coumarate/ferulate ratio, and other ending structures. The results also indicated that approximately 8% of mass weight was extracted by pure ethanol. The bagasse after ethanol extraction had an approximate 22% higher glucose yield after enzyme hydrolysis compared to pretreated bagasse without extraction. Copyright © 2013 Elsevier Ltd. All rights reserved.

  4. Pretreatment of moso bamboo with dilute phosphoric acid

    Directory of Open Access Journals (Sweden)

    Bo Hong


    Full Text Available Dilute phosphoric acid pretreatment of moso bamboo materials was studied for producing high quality dissolving pulp for textile applications. The dynamics of dilute acid pretreatment were considered. The Saeman model was found to describe well the acid hydrolysis of moso bamboo hemicelluloses to their monomers under different temperatures and different dilute phosphoric acid concentrations. The initial degradation rate of hemicelluloses was much higher than its subsequent degradation rate, and the xylose generation rate increased with increasing temperature. The change rule of the pentose extraction rate was considered along with the pretreatment factor (P factor. Optimum dilute acid pretreatment conditions were 170 °C and 45 minutes. Based on the optimum conditions and a mass balance of sugars, a weight loss of 26.5% of the solid and liquid fractions combined was observed after the pretreatment. SEM results revealed that the moso bamboo fibers surfaces and cell wall were damaged. With the surface area increasing, the accessible pore areas also increased. At the same time, the crystallinity of the cellulose was reduced, which created a favorable environment for chemical penetration in the subsequent treatment.

  5. Measurement of pyrethroid, organophosphorus, and carbamate insecticides in human plasma using isotope dilution gas chromatography-high resolution mass spectrometry. (United States)

    Pérez, José J; Williams, Megan K; Weerasekera, Gayanga; Smith, Kimberly; Whyatt, Robin M; Needham, Larry L; Barr, Dana Boyd


    We have developed a gas chromatography-high resolution mass spectrometry method for measuring pyrethroid, organophosphorus, carbamate and fipronil pesticides and the synergist piperonyl butoxide in human plasma. Plasma samples were extracted using solid phase extraction and were then concentrated for injection and analysis using isotope dilution gas chromatography-high resolution mass spectrometry. The limits of detection ranged from 10 to 158 pg/mL with relative recoveries at concentrations near the LODs (e.g., 25 or 250 pg/mL) ranging from 87% to 156% (9 of the 16 compounds were within ±15% of 100%). The extraction recoveries ranged from 20% to 98% and the overall method relative standard deviations were typically less than 20% with some exceptions. Analytical characteristics were determined at 25, 250, and 1000 pg/mL.

  6. Removal of iron interferences by solvent extraction for geochemical analysis by atomic-absorption spectrophotometry (United States)

    Zhou, L.; Chao, T.T.; Sanzolone, R.F.


    Iron is a common interferent in the determination of many elements in geochemical samples. Two approaches for its removal have been taken. The first involves removal of iron by extraction with methyl isobutyl ketone (MIBK) from hydrochloric acid medium, leaving the analytes in the aqueous phase. The second consists of reduction of iron(III) to iron(II) by ascorbic acid to minimize its extraction into MIBK, so that the analytes may be isolated by extraction. Elements of interest can then be determined using the aqueous solution or the organic extract, as appropriate. Operating factors such as the concentration of hydrochloric acid, amounts of iron present, number of extractions, the presence or absence of a salting-out agent, and the optimum ratio of ascorbic acid to iron have been determined. These factors have general applications in geochemical analysis by atomic-absorption spectrophotometry. ?? 1985.

  7. Suitability of stem latex of jatropha gossypifolia as a protein precipitant for biochemical analysis. (United States)

    Adeosun, O G; Oduola, T; Fagbomedo, F A; Oyedeji, S O; Akanji, B O; Adesina, A A


    The extract of Jatropha Gossypifolia stem was obtained by cutting the stem with a sharp knife and the fluid expressed out. The suitability of the stem latex extract as a precipitant for biochemical analysis was determined. The precipitating efficacy of the extract for creatinine and protein estimation was found to be optimum at 1/4 and 1/5 dilutions respectively aqueous solution. Plasma protein was precipitated with stem extract of J. Gossypifolia at the stated dilution. The mean plasma creatinine values obtained from 0.5 % sodium tungstate as a protein precipitant were compared with the values of plasma creatinine obtained when ¼ dilution of stem extract of J. Gossypifolia was used as protein precipitant. Similarly mean cerebrospinal fluid (CSF) and urinary protein values obtained from 3 % Tricholoro-acetic acid as protein precipitant were compared with values obtained from 1/5 dilution of stem extract of J. Gossypifolia as protein precipitant. The values obtained from the stem latex extract at the stated dilutions were comparable with values obtained from the conventional protein precipitants (p < 0.05). The stem latex extract of J. Gossypifolia is suitable as a protein precipitant for creatinine, CSF and urinary protein estimations. However further work need to be done to purify the extract and determine the exact concentration at the stated dilutions as well as the active ingredient in stem latex.

  8. Optimising the Use of TRIzol-extracted Proteins in Surface Enhanced Laser Desorption/ Ionization (SELDI Analysis

    Directory of Open Access Journals (Sweden)

    Perlaky Laszlo


    Full Text Available Abstract Background Research with clinical specimens is always hampered by the limited availability of relevant samples, necessitating the use of a single sample for multiple assays. TRIzol is a common reagent for RNA extraction, but DNA and protein fractions can also be used for other studies. However, little is known about using TRIzol-extracted proteins in proteomic research, partly because proteins extracted from TRIzol are very resistant to solubilization. Results To facilitate the use of TRIzol-extracted proteins, we first compared the ability of four different common solubilizing reagents to solubilize the TRIzol-extracted proteins from an osteosarcoma cell line, U2-OS. Then we analyzed the solubilized proteins by Surface Enhanced Laser Desorption/ Ionization technique (SELDI. The results showed that solubilization of TRIzol-extracted proteins with 9.5 M Urea and 2% CHAPS ([3-[(3-cholamidopropyl-dimethylammonio]propanesulfonate] (UREA-CHAPS was significantly better than the standard 1% SDS in terms of solubilization efficiency and the number of detectable ion peaks. Using three different types of SELDI arrays (CM10, H50, and IMAC-Cu, we demonstrated that peak detection with proteins solubilized by UREA-CHAPS was reproducible (r > 0.9. Further SELDI analysis indicated that the number of ion peaks detected in TRIzol-extracted proteins was comparable to a direct extraction method, suggesting many proteins still remain in the TRIzol protein fraction. Conclusion Our results suggest that UREA-CHAPS performed very well in solubilizing TRIzol-extracted proteins for SELDI applications. Protein fractions left over after TRIzol RNA extraction could be a valuable but neglected source for proteomic or biochemical analysis when additional samples are not available.

  9. Phytochemical analysis and standardization of Strychnos nux-vomica extract through HPTLC techniques

    Directory of Open Access Journals (Sweden)

    Dinesh Kumar Patel


    Full Text Available Objective: The objective is to develop a noval qualitative and quantitative method by which we can determine different phytoconstituents of Strychnos nux-vomica L. Methods: To profile the phyconstituents of Strychnos nux-vomica, in the present study hydroalcoholic extract of Strychnos nux-vomica was subjected to preliminary phytochemical analysis, antimicrobial activities against certain pathogenic microorganisms, solubility test, loss on drying and pH value. Extract was also subjected to the quantitative analysis including total phenol, flavonoid and heavy metal analysis. Quantitative analysis was performed through HPTLC methods using strychnine and brucine as a standard marker. Results: Phytochemical analysis revealed the presence of alkaloid, carbohydrate, tannin, steroid, triterpenoid and glycoside in the extract. Total flavonoid and phenol content of Strychnos nux-vomica L extract was found to be 0.40 % and 0.43%. Result showed that the level of heavy metal (lead, arsenic, mercury and cadmium complie the standard level. Total bacterial count, yeast and moulds contents were found to be under the limit whereas E. coli and salmonella was found to be absent in the extract. Content of strychnine and brucine were found to be 4.75% and 3.91%. Conclusions: These studies provide valluable information for correct identification and selection of the drug from various adulterations. In future this study will be helpful for the quantitative analysis as well as standardization of the Strychnos nux-vomica L.


    Directory of Open Access Journals (Sweden)

    C. Baskaran


    Full Text Available To investigate the antimicrobial activity and phytochemical screening Ethanol, methanol, Ethyl acetate, aceton,chloroform, Petroleum ether, hexane, hot water, and extracts of Murraya koenigii. The aim of the present study was to evaluate the qualitative analysis of phytochemicals and antimicrobial activity of various solvent extracts of Murraya koenigii. The antimicrobial activity of different solvent extracts of Murraya koenigii were tested against the Gram-positive and Gram-negative bacterial strains and fungus by observing the zone of inhibition. The Gram-positive bacteria used in the test were Staphylococcus aureus, Bacillus cereus and Micrococcus luteus, and the Gram-negative bacteria were Escherichia coli, Pseudomonas aeruginosa and Klebsiella pneumoniae, fungus like Aspergillus niger, Candida albicans, Candida tropicalis, Cryptococcus neoformans and Candida kefyr. It was observed that ethanol, methanol, ethyl acetate, aceton, chloroform, petroleum ether, hexane and aquas extracts showed activity against bacteria and fungus. The Hot water extract of Murraya koenigii showed more activity against Staphylococcus aureus, zone of diameter 28.17±0.29mm and Ethanol extract of Murraya koenigii showed more activity against Aspergillus niger and Candida tropicalis, zone of diameter 12.17±0.15mm compared to other solvent extracts. In this study Hot water Extract in bacteria and Ethanol Extract in fungus showed a varying degree of inhibition to the growth of tested organism, than methanol, Ethyl acetate, aceton, chloroform, Petroleum ether, hexane, and acetone extracts, The results confirmed the presence of antibacterial activity of Murraya koenigii extract against various human pathogenic bacteria. Presences of phytochemical and antimicrobial activity are confirmed.

  11. Comparative and quantitative analysis of antioxidant and scavenging potential of Indigofera tinctoria Linn. extracts

    Institute of Scientific and Technical Information of China (English)

    Rashmi Singh; Shatruhan Sharma; Veena Sharma


    OBJECTIVE: To compare and elucidate the antioxidant efifcacy of ethanolic and hydroethanolic extracts ofIndigofera tinctoriaLinn. (Fabaceae family). METHODS: Variousin-vitro antioxidant assays and free radical-scavenging assays were done. Quantitative measurements of various phytoconstituents, reductive abilities and chelating potential were carried out along with standard compounds. Half inhibitory concentration (IC50) values for ethanol and hydroethanol extracts were analyzed and compared with respective standards. RESULTS: Hydroethanolic extracts showed considerably more potent antioxidant activity in comparison to ethanol extracts. Hydroethanolic extracts had lower IC50 values than ethanol extracts in the case of DPPH, metal chelation and hydroxyl radical-scavenging capacity (829, 659 and 26.7 μg/mL) but had slightly higher values than ethanol in case of SO2- and NO2-scavenging activity (P< 0.001vs standard). Quantitative measurements also showed that the abundance of phenolic and lfavonoid bioactive phytoconstituents were signiifcantly (P< 0.001) greater in hydroethanol extracts (212.920 and 149.770 mg GAE and rutin/g of plant extract respectively) than in ethanol extracts (211.691 and 132.603 mg GAE and rutin/g of plant extract respectively). Karl Pearson’s correlation analysis (r2) between various antioxidant parameters and bioactive components also associated the antioxidant potential ofI. tinctoria with various phytoconstituents, especialy phenolics, lfavonoids, saponins and tannins. CONCLUSION: This study may be helpful to draw the attention of researchers towards the hydroethanol extracts ofI. tinctoria, which has a high yield, and great prospects in herbal industries to produce inexpensive and powerful herbal products.

  12. Analysis of Volatile Compounds from Solanumbetaceum Cav. Fruits from Panama by Head-Space Micro Extraction

    Directory of Open Access Journals (Sweden)

    Armando A. Durant


    Full Text Available The characterization of the volatile compounds of two varieties of Solanum betaceum Cav. by means of headspace solid-phase microextraction (HS-SPME coupled with gas chromatography-mass spectrometry ( GC-MS i s presented. The HS-SPME method for extraction of the volatiles compounds was optimized by using a 2 3 central composite design. Maximum extraction of volatile compounds was achieved by using a divinylbenzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS fiber, extraction temperature 76° C, incubation time 44 min, and extraction time of 46 min. The main types of compounds detected in both varieties are terpenoids, followed by aromatics, esters, and aldehydes. Golden-yellow cultivars contained higher levels of esters and terpenes, while the reddish-purple variety contained a significant amount of aromatic compounds. The data structure of the chemical information obtained as well as the relationship between variables was evaluated by means of principal component analysis and cluster analysis.

  13. Texture features analysis for coastline extraction in remotely sensed images (United States)

    De Laurentiis, Raimondo; Dellepiane, Silvana G.; Bo, Giancarlo


    The accurate knowledge of the shoreline position is of fundamental importance in several applications such as cartography and ships positioning1. Moreover, the coastline could be seen as a relevant parameter for the monitoring of the coastal zone morphology, as it allows the retrieval of a much more precise digital elevation model of the entire coastal area. The study that has been carried out focuses on the development of a reliable technique for the detection of coastlines in remotely sensed images. An innovative approach which is based on the concepts of fuzzy connectivity and texture features extraction has been developed for the location of the shoreline. The system has been tested on several kind of images as SPOT, LANDSAT and the results obtained are good. Moreover, the algorithm has been tested on a sample of a SAR interferogram. The breakthrough consists in the fact that the coastline detection is seen as an important features in the framework of digital elevation model (DEM) retrieval. In particular, the coast could be seen as a boundary line all data beyond which (the ones representing the sea) are not significant. The processing for the digital elevation model could be refined, just considering the in-land data.

  14. Composition analysis and antioxidant properties of black garlic extract

    Directory of Open Access Journals (Sweden)

    Xiaoming Lu


    Full Text Available Black garlic produced from fresh garlic under controlled high temperature and humidity has strong antioxidant properties. To determine these compounds, five fractions (from F1 to F5 were separated and purified by elution with chloroform:methanol at different ratios (8:1, 6:1, 4:1, 2:1, and 0:1; v/v. The antioxidant activity of each fraction was analyzed. The results showed that F3 and F4 had higher phenolic contents and stronger 2,2-diphenyl-2-picrylhydrazyl radical scavenging activity than the others. Seven purified individual components were further separated using semipreparation high-performance liquid chromatography from these two intensely antioxidant fractions (F3 and F4, their structures were elucidated by high-performance liquid chromatography coupled to diode array detection, electrospray ionization, mass spectrometry, 1H nuclear magnetic resonance, and 13C nuclear magnetic resonance spectrometry. Three compounds including adenosine, uridine, and 2-acetylpyrrole were first identified in black garlic, except for 5-hydroxymethylfurfural, (1S, 3S-1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid, and (1R, 3S-1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid. The cellular antioxidant activities of uridine, adenosine, carboline alkaloids, 5-hydroxymethylfurfural, and ethyl acetate extracts were consistent with the results of in vitro experimental antioxidant properties. The results provide useful information for understanding the health benefits of black garlic products.

  15. A risk-based approach to management of leachables utilizing statistical analysis of extractables. (United States)

    Stults, Cheryl L M; Mikl, Jaromir; Whelehan, Oliver; Morrical, Bradley; Duffield, William; Nagao, Lee M


    To incorporate quality by design concepts into the management of leachables, an emphasis is often put on understanding the extractable profile for the materials of construction for manufacturing disposables, container-closure, or delivery systems. Component manufacturing processes may also impact the extractable profile. An approach was developed to (1) identify critical components that may be sources of leachables, (2) enable an understanding of manufacturing process factors that affect extractable profiles, (3) determine if quantitative models can be developed that predict the effect of those key factors, and (4) evaluate the practical impact of the key factors on the product. A risk evaluation for an inhalation product identified injection molding as a key process. Designed experiments were performed to evaluate the impact of molding process parameters on the extractable profile from an ABS inhaler component. Statistical analysis of the resulting GC chromatographic profiles identified processing factors that were correlated with peak levels in the extractable profiles. The combination of statistically significant molding process parameters was different for different types of extractable compounds. ANOVA models were used to obtain optimal process settings and predict extractable levels for a selected number of compounds. The proposed paradigm may be applied to evaluate the impact of material composition and processing parameters on extractable profiles and utilized to manage product leachables early in the development process and throughout the product lifecycle.

  16. Supercritical Fluid Extraction of Quinones from Compost for Microbial Community Analysis

    Directory of Open Access Journals (Sweden)

    Ni Luh Gede Ratna Juliasih


    Full Text Available Supercritical fluid extraction (SFE was used to extract quinones from compost to monitor the microbial community dynamics during composting. The 0.3 g of dried compost was extracted using 3 mL min−1 of carbon dioxide (90% and methanol (10% at 45°C and 25 MPa for a 30 min extraction time. The extracted quinones were analysed using ultra performance liquid chromatography (UPLC with 0.3 mL min−1 of methanol mobile phase for a 50 min chromatographic run time. A comparable detected amount of quinones was obtained using the developed method and an organic solvent extraction method, being 36.06 μmol kg−1 and 34.54 μmol kg−1, respectively. Significantly low value of dissimilarity index (D between the two methods (0.05 indicated that the quinone profile obtained by both methods was considered identical. The developed method was then applied to determine the maturity of the compost by monitoring the change of quinone during composting. The UQ-9 and MK-7 were predominant quinones in the initial stage of composting. The diversity of quinone became more complex during the cooling and maturation stages. This study showed that SFE had successfully extracted quinones from a complex matrix with simplification and rapidity of the analysis that is beneficial for routine analysis.

  17. Large datasets: Segmentation, feature extraction, and compression

    Energy Technology Data Exchange (ETDEWEB)

    Downing, D.J.; Fedorov, V.; Lawkins, W.F.; Morris, M.D.; Ostrouchov, G.


    Large data sets with more than several mission multivariate observations (tens of megabytes or gigabytes of stored information) are difficult or impossible to analyze with traditional software. The amount of output which must be scanned quickly dilutes the ability of the investigator to confidently identify all the meaningful patterns and trends which may be present. The purpose of this project is to develop both a theoretical foundation and a collection of tools for automated feature extraction that can be easily customized to specific applications. Cluster analysis techniques are applied as a final step in the feature extraction process, which helps make data surveying simple and effective.

  18. FY12 Final Report for PL10-Mod Separations-PD12: Electrochemically Modulated Separation of Plutonium from Dilute and Concentrated Dissolver Solutions for Analysis by Gamma Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Pratt, Sandra H.; Arrigo, Leah M.; Duckworth, Douglas C.; Cloutier, Janet M.; Breshears, Andrew T.; Schwantes, Jon M.


    Accurate and timely analysis of plutonium in spent nuclear fuel is critical in nuclear safeguards for detection of both protracted and rapid plutonium diversions. Gamma spectroscopy is a viable method for accurate and timely measurements of plutonium provided that the plutonium is well separated from the interfering fission and activation products present in spent nuclear fuel. Electrochemically modulated separation (EMS) is a method that has been used successfully to isolate picogram amounts of Pu from nitric acid matrices. With EMS, Pu adsorption may be turned “on” and “off” depending on the applied voltage, allowing for collection and stripping of Pu without the addition of chemical reagents. In this work, we have scaled up the EMS process to isolate microgram quantities of Pu from matrices encountered in spent nuclear fuel during reprocessing. Several challenges have been addressed including surface area limitations, radiolysis effects, electrochemical cell performance stability, and chemical interferences. After these challenges were resolved, 6 µg Pu was deposited in the electrochemical cell with approximately an 800-fold reduction of fission and activation product levels from a spent nuclear fuel sample. Modeling showed that these levels of Pu collection and interference reduction may not be sufficient for Pu detection by gamma spectroscopy. The main remaining challenges are to achieve a more complete Pu isolation and to deposit larger quantities of Pu for successful gamma analysis of Pu. If gamma analyses of Pu are successful, EMS will allow for accurate and timely on-site analysis for enhanced Pu safeguards.

  19. Secondary Metabolites Analysis of Methanol Extract of Surian (Toona sureni (Bl. Merr Leaf as Antioxidant Potential.

    Directory of Open Access Journals (Sweden)



    Full Text Available Secondary Metabolites Analysis of Methanol Extract of Surian (Toona sureni (Bl. Merr Leaf as AntioxidantPotential. The study of performed secondary metabolites from the methanol extract of Surian (Toona sureni (Bl. Merrleaves have been done by thin-layer chromatography (TLC method. The result showed that methanol extract of Surianleaves consist of alkaloid, flavonoid, polyphenol and terpenoid. All of them positively have the ability to scavenge 2,2-diphenyl-1-picrylhydrazyl (DPPH. It has IC50 (4.80 are smaller than the ascorbat acid standard (IC50 = 9.23.

  20. The Anisotropic Transport Effects On The Dilute Plasmas

    CERN Document Server

    Devlen, Ebru


    We examine the linear stability analysis of a hot, dilute and differentially rotating plasma by considering anisotropic transport effects. In the dilute plasmas, the ion Larmor radius is small compared with its collisional mean free path. In this case, the transport of heat and momentum along the magnetic field lines become important. This paper presents a novel linear instability that may more powerful and greater than ideal magnetothermal instability (MTI) and ideal magnetorotational instability (MRI) in the dilute astrophysical plasmas. This type of plasma is believed to be found in the intracluster medium of galaxy clusters and radiatively ineffective accretion flows around black holes. We derive the dispersion relation of this instability and obtain the instability condition. There is at least one unstable mode that is independent of the temperature gradient direction for a helical magnetic field geometry. This novel instability is driven by the gyroviscosity coupled with differential rotation. Therefore...

  1. Analysis of sampling artifacts on the Granger causality analysis for topology extraction of neuronal dynamics. (United States)

    Zhou, Douglas; Zhang, Yaoyu; Xiao, Yanyang; Cai, David


    Granger causality (GC) is a powerful method for causal inference for time series. In general, the GC value is computed using discrete time series sampled from continuous-time processes with a certain sampling interval length τ, i.e., the GC value is a function of τ. Using the GC analysis for the topology extraction of the simplest integrate-and-fire neuronal network of two neurons, we discuss behaviors of the GC value as a function of τ, which exhibits (i) oscillations, often vanishing at certain finite sampling interval lengths, (ii) the GC vanishes linearly as one uses finer and finer sampling. We show that these sampling effects can occur in both linear and non-linear dynamics: the GC value may vanish in the presence of true causal influence or become non-zero in the absence of causal influence. Without properly taking this issue into account, GC analysis may produce unreliable conclusions about causal influence when applied to empirical data. These sampling artifacts on the GC value greatly complicate the reliability of causal inference using the GC analysis, in general, and the validity of topology reconstruction for networks, in particular. We use idealized linear models to illustrate possible mechanisms underlying these phenomena and to gain insight into the general spectral structures that give rise to these sampling effects. Finally, we present an approach to circumvent these sampling artifacts to obtain reliable GC values.

  2. Analysis of Sampling Artifacts on the Granger Causality Analysis for Topology Extraction of Neuronal Dynamics

    Directory of Open Access Journals (Sweden)

    Douglas eZhou


    Full Text Available Granger causality (GC is a powerful method for causal inference for time series. In general, the GC value is computed using discrete time series sampled from continuous-time processes with a certain sampling interval length $tau$, emph{i.e.}, the GC value is a function of $tau$. Using the GC analysis for the topology extraction of the simplest integrate-and-fire neuronal network of two neurons, we discuss behaviors of the GC value as a function of $tau$, which exhibits (i oscillations, often vanishing at certain finite sampling interval lengths, (ii the GC vanishes linearly as one uses finer and finer sampling. We show that these sampling effects can occur in both linear and nonlinear dynamics: the GC value may vanish in the presence of true causal influence or become nonzero in the absence of causal influence. Without properly taking this issue into account, GC analysis may produce unreliable conclusions about causal influence when applied to empirical data. These sampling artifacts on the GC value greatly complicate the reliability of causal inference using the GC analysis, in general, and the validity of topology reconstruction for networks, in particular. We use idealized linear models to illustrate possible mechanisms underlying these phenomena and to gain insight into the general spectral structures that give rise to these sampling effects. Finally, we present an approach to circumvent these sampling artifacts to obtain reliable GC values.


    Institute of Scientific and Technical Information of China (English)

    Li Shugang


    Coalbed methane is of great value to extract and utilize in China, but the result of such research is not satisfied yet today.The paper analyzed the storage characteristics of coalbed methane, and then studied the behavior of coalbed methane using the key stratum theory of strata control.According to the features related to coalbed methane accumulations and delivery, the technique for safely simultaneous extraction of coal and coalbed methane is proposed, and benefit analysis is made too.

  4. Hydrometallurgical process for zinc recovery from electric arc furnace dust (EAFD): part I: Characterization and leaching by diluted sulphuric acid. (United States)

    Oustadakis, P; Tsakiridis, P E; Katsiapi, A; Agatzini-Leonardou, S


    The present paper is the first of a series of two articles dealing with the development of an integrated process for the recovery of zinc from electric arc furnace dust (EAFD), a hazardous industrial waste generated in the collection of particulate material during steelmaking process via electric arc furnace. Part I presents the EAFD characterization and its leaching process by diluted sulphuric acid, whereas Part II deals with the purification of the leach liquor and the recovery of zinc by solvent extraction/electrowinning. The characterization of the examined electric arc furnace dust was carried out by using granulometry analysis, chemical analysis, X-ray diffraction (XRD), thermogravimetric/differential thermal analysis (TG/DTA) and scanning electron microscopy (SEM). The leaching process was based on the Zn extraction with diluted sulphuric acid from EAFD under atmospheric conditions and without using any preliminary treatment. Statistical design and analysis of experiments were used, in order to determine the main effects and interactions of the leaching process factors, which were: acid normality, temperature and solid to liquid ratio. The zinc recovery efficiency on the basis of EAFD weight reached 80%. X-ray diffraction and scanning electron microscopy were used for the characterization of the leached residues.

  5. Liquid membrane extraction techniques for trace metal analysis and speciation in environmental and biological matrices

    Energy Technology Data Exchange (ETDEWEB)

    Ndungu, Kuria


    In this thesis, liquid-membrane-based methods for the analysis of trace metal species in samples of environmental and biological origin were developed. By incorporating extracting reagents in the membrane liquid, trace metal ions were selectively separated from humic-rich natural waters and urine samples, prior to their determination using various instrumental techniques. The extractions were performed in closed flow systems thus allowing easy automation of both the sample clean-up and enrichment. An acidic organophosphorus reagent (DEHPA) and a basic tetraalkylammonium reagent (Aliquat-336) were used as extractants in the membrane liquid to selectively extract and enrich cationic and anionic metal species respectively. A speciation method for chromium species was developed that allowed the determination of cationic Cr(III) species and anionic CR(VI) species in natural water samples without the need of a chromatographic separation step prior to their detection. SLM was also coupled on-line to potentiometric stripping analysis providing a fast and sensitive method for analysis of Pb in urine samples. A microporous membrane liquid-liquid extraction (MMLLE) method was developed for the determination of organotin compounds in natural waters that reduced the number of manual steps involved in the LLE of organotin compounds prior to their CC separation. Clean extracts obtained after running unfiltered humic-rich river water samples through the MMLLE flow system allowed selective determination of all the organotin compounds in a single run using GC-MS in the selected ion monitoring mode (SIM) 171 refs, 9 figs, 4 tabs

  6. Composition analysis and antioxidant properties of black garlic extract. (United States)

    Lu, Xiaoming; Li, Ningyang; Qiao, Xuguang; Qiu, Zhichang; Liu, Pengli


    Black garlic produced from fresh garlic under controlled high temperature and humidity has strong antioxidant properties. To determine these compounds, five fractions (from F1 to F5) were separated and purified by elution with chloroform:methanol at different ratios (8:1, 6:1, 4:1, 2:1, and 0:1; v/v). The antioxidant activity of each fraction was analyzed. The results showed that F3 and F4 had higher phenolic contents and stronger 2,2-diphenyl-2-picrylhydrazyl radical scavenging activity than the others. Seven purified individual components were further separated using semipreparation high-performance liquid chromatography from these two intensely antioxidant fractions (F3 and F4), their structures were elucidated by high-performance liquid chromatography coupled to diode array detection, electrospray ionization, mass spectrometry, (1)H nuclear magnetic resonance, and (13)C nuclear magnetic resonance spectrometry. Three compounds including adenosine, uridine, and 2-acetylpyrrole were first identified in black garlic, except for 5-hydroxymethylfurfural, (1S, 3S)-1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid, and (1R, 3S)-1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid. The cellular antioxidant activities of uridine, adenosine, carboline alkaloids, 5-hydroxymethylfurfural, and ethyl acetate extracts were consistent with the results of in vitro experimental antioxidant properties. The results provide useful information for understanding the health benefits of black garlic products. Copyright © 2016. Published by Elsevier B.V.


    Directory of Open Access Journals (Sweden)

    Alexander Vatľák


    Full Text Available The aim of this study was antimicrobial action of the methanolic extracts of Equisetum arvense L. and Urtica dioica L. against gramnegative and grampositive bacteria. The antimicrobial activities of the extracts against gramnegative bacteria: Escherichia coli CCM 3988, Listeria ivanovii CCM 5884, Listeria innocua CCM 4030, Pseudomonas aeruginosa CCM 1960, Serratia rubidaea CCM 4684 and grampositive bacteria: Brochothrix thermosphacta CCM 4769, Enterococcus raffinosus CCM 4216, Lactobacillus rhamnosus CCM 1828, Paenobacillus larvae CCM 4483 and Staphylococcus epidermis CCM 4418 were determined by the disc diffusion method and the microbroth dilution method according to CLSI. Probit analysis was used in this experiment. Of the 2 plant extracts tested, all extracts showed antimicrobial activity against one or more species of microorganisms. The most antimicrobial activity showed methanolic plant extract of E. arvense against S. epidermis with disc diffusion method and with microbroth dilution method against S. rubidaea and plant extract Urtica dioica with disc diffusion method against P. aeruginosa and with microbroth dilution method against S. rubidaea and E. coli.

  8. Fast and solvent-free quantitation of boar taint odorants in pig fat by stable isotope dilution analysis-dynamic headspace-thermal desorption-gas chromatography/time-of-flight mass spectrometry. (United States)

    Fischer, Jochen; Haas, Torsten; Leppert, Jan; Lammers, Peter Schulze; Horner, Gerhard; Wüst, Matthias; Boeker, Peter


    Boar taint is a specific off-odour of boar meat products, known to be caused by at least three unpleasant odorants, with very low odour thresholds. Androstenone is a boar pheromone produced in the testes, whereas skatole and indole originate from the microbial breakdown of tryptophan in the intestinal tract. A new procedure, applying stable isotope dilution analysis (SIDA) and dynamic headspace-thermal desorption-gas chromatography/time-of-flight mass spectrometry (dynHS-TD-GC/TOFMS) for the simultaneous quantitation of these boar taint compounds in pig fat was elaborated and validated in this paper. The new method is characterised by a simple and solvent-free dynamic headspace sampling. The deuterated compounds d3-androstenone, d3-skatole and d6-indole were used as internal standards to eliminate matrix effects. The method validation performed revealed low limits of detection (LOD) and quantitation (LOQ) with high accuracy and precision, thus confirming the feasibility of the new dynHS-TD-GC/TOFMS approach for routine analysis.

  9. Determination of Characteristic Components in Essential Oils from Wisteria brachybotrys Using Gas Chromatography-Olfactometry Incremental Dilution Technique

    Directory of Open Access Journals (Sweden)

    Mitsuo Miyazawa


    Full Text Available The essential oil, obtained by steam distillation of flowers, leaves and stems from Wisteria brachybotrys Zucc, collected in Japan was analyzed by gas chromatography (GC and GC-MS. The important aroma-active compounds were also detected in the oil using GC-MS/Olfactometry (GC-MS/O and aroma extraction dilution analysis (AEDA. As a result, sixty-eight compounds from flowers of W. brachybotrys, accounting for 96.3%, were identified, and benzyl cyanide (31.7%, palmitic acid (8.7%, and (Z- g -bisabolene (8.4% as the main compounds. Thirty compounds from leaves, accounting for 97.3%, were identified, and phytol (46.0%, palmitic acid (8.2%, and nonanal (5.7% as the main compounds. Twenty-eight compounds from stems, accounting for 98.7%, were identified, and geraniol (32.8%, linalool (22.1%, and nerol (10.4% as the main compounds. A preliminary analysis by GC-MS and using Kovats’ retention indexes, lead to characterize and quantify the oil constituents, while GC-MS/O was then applied for the identification of the main odorants. By the incremental dilution method (AEDA, applied to the GC-MS/O technique, the flavor dilution (FD factor was obtained. To our knowledge, the composition of these parts of essential oils is described here for the first time, both from the chemical and olfactometric viewpoints.

  10. Streamlined Membrane Proteome Preparation for Shotgun Proteomics Analysis with Triton X-100 Cloud Point Extraction and Nanodiamond Solid Phase Extraction

    Directory of Open Access Journals (Sweden)

    Minh D. Pham


    Full Text Available While mass spectrometry (MS plays a key role in proteomics research, characterization of membrane proteins (MP by MS has been a challenging task because of the presence of a host of interfering chemicals in the hydrophobic protein extraction process, and the low protease digestion efficiency. We report a sample preparation protocol, two-phase separation with Triton X-100, induced by NaCl, with coomassie blue added for visualizing the detergent-rich phase, which streamlines MP preparation for SDS-PAGE analysis of intact MP and shot-gun proteomic analyses. MP solubilized in the detergent-rich milieu were then sequentially extracted and fractionated by surface-oxidized nanodiamond (ND at three pHs. The high MP affinity of ND enabled extensive washes for removal of salts, detergents, lipids, and other impurities to ensure uncompromised ensuing purposes, notably enhanced proteolytic digestion and down-stream mass spectrometric (MS analyses. Starting with a typical membranous cellular lysate fraction harvested with centrifugation/ultracentrifugation, MP purities of 70%, based on number (not weight of proteins identified by MS, was achieved; the weight-based purity can be expected to be much higher.

  11. Simultaneous analysis of cortisol and cortisone in saliva using XLC-MS/MS for fully automated online solid phase extraction. (United States)

    Jones, Rachel L; Owen, Laura J; Adaway, Joanne E; Keevil, Brian G


    Salivary cortisol measurements are increasingly being used in the investigation of disorders of the hypothalamic-pituitary-adrenal axis. In the salivary gland, cortisol is metabolised to cortisone by the action of 11β-hydroxysteroid dehydrogenase type 2, and cortisone is partly responsible for the variable interference observed in current salivary cortisol immunoassays. The aim of this study was to validate an assay for the simultaneous analysis of salivary cortisol and cortisone using the Spark Holland Symbiosis™ in eXtraction liquid chromatography-tandem mass spectrometry (XLC-MS/MS) mode for fully automated online solid phase extraction (SPE). Saliva samples were diluted in water with the addition of internal standard (d4-cortisol and d7-cortisone). Online SPE was performed using the Spark Holland Symbiosis™ with HySphere™ C18 SPE cartridges and compounds were eluted onto a Phenomenex® C18 guard column attached to a Phenomenex® Onyx monolithic C18 column for chromatography. Mass spectrometry used the Waters® Xevo™ TQ MS in electrospray positive mode. Cortisol and cortisone eluted with their internal standards at 1.95 and 2.17 min, respectively, with a total run time of four minutes. No evidence of ion-suppression was observed. The assay was linear up to 3393 nmol/L for cortisol and 3676 nmol/L for cortisone, with lower limits of quantitation of 0.75 nmol/L and 0.50 nmol/L, respectively. Intra- and inter-assay imprecision was cortisone across three levels of internal quality control, with accuracy and recovery within accepted limits. High specificity was demonstrated following interference studies which assessed 29 structurally-related steroids at supra-physiological concentrations. We have successfully validated an assay for the simultaneous analysis of salivary cortisol and cortisone using XLC-MS/MS and fully automated online SPE. The assay benefits from increased specificity compared to immunoassay and minimal sample preparation which allows high

  12. Extraction of DNA by magnetic ionic liquids: tunable solvents for rapid and selective DNA analysis. (United States)

    Clark, Kevin D; Nacham, Omprakash; Yu, Honglian; Li, Tianhao; Yamsek, Melissa M; Ronning, Donald R; Anderson, Jared L


    DNA extraction represents a significant bottleneck in nucleic acid analysis. In this study, hydrophobic magnetic ionic liquids (MILs) were synthesized and employed as solvents for the rapid and efficient extraction of DNA from aqueous solution. The DNA-enriched microdroplets were manipulated by application of a magnetic field. The three MILs examined in this study exhibited unique DNA extraction capabilities when applied toward a variety of DNA samples and matrices. High extraction efficiencies were obtained for smaller single-stranded and double-stranded DNA using the benzyltrioctylammonium bromotrichloroferrate(III) ([(C8)3BnN(+)][FeCl3Br(-)]) MIL, while the dicationic 1,12-di(3-hexadecylbenzimidazolium)dodecane bis[(trifluoromethyl)sulfonyl]imide bromotrichloroferrate(III) ([(C16BnIM)2C12(2+)][NTf2(-), FeCl3Br(-)]) MIL produced higher extraction efficiencies for larger DNA molecules. The MIL-based method was also employed for the extraction of DNA from a complex matrix containing albumin, revealing a competitive extraction behavior for the trihexyl(tetradecyl)phosphonium tetrachloroferrate(III) ([P6,6,6,14(+)][FeCl4(-)]) MIL in contrast to the [(C8)3BnN(+)][FeCl3Br(-)] MIL, which resulted in significantly less coextraction of albumin. The MIL-DNA method was employed for the extraction of plasmid DNA from bacterial cell lysate. DNA of sufficient quality and quantity for polymerase chain reaction (PCR) amplification was recovered from the MIL extraction phase, demonstrating the feasibility of MIL-based DNA sample preparation prior to downstream analysis.

  13. Topology analysis of social networks extracted from literature. (United States)

    Waumans, Michaël C; Nicodème, Thibaut; Bersini, Hugues


    In a world where complex networks are an increasingly important part of science, it is interesting to question how the new reading of social realities they provide applies to our cultural background and in particular, popular culture. Are authors of successful novels able to reproduce social networks faithful to the ones found in reality? Is there any common trend connecting an author's oeuvre, or a genre of fiction? Such an analysis could provide new insight on how we, as a culture, perceive human interactions and consume media. The purpose of the work presented in this paper is to define the signature of a novel's story based on the topological analysis of its social network of characters. For this purpose, an automated tool was built that analyses the dialogs in novels, identifies characters and computes their relationships in a time-dependent manner in order to assess the network's evolution over the course of the story.

  14. Topology analysis of social networks extracted from literature.

    Directory of Open Access Journals (Sweden)

    Michaël C Waumans

    Full Text Available In a world where complex networks are an increasingly important part of science, it is interesting to question how the new reading of social realities they provide applies to our cultural background and in particular, popular culture. Are authors of successful novels able to reproduce social networks faithful to the ones found in reality? Is there any common trend connecting an author's oeuvre, or a genre of fiction? Such an analysis could provide new insight on how we, as a culture, perceive human interactions and consume media. The purpose of the work presented in this paper is to define the signature of a novel's story based on the topological analysis of its social network of characters. For this purpose, an automated tool was built that analyses the dialogs in novels, identifies characters and computes their relationships in a time-dependent manner in order to assess the network's evolution over the course of the story.

  15. Large Scale Data Analysis and Knowledge Extraction in Communication Data (United States)


    problem [11 ,12] Examples of important applications include characterizing potential candidates for viral marketing , finding members of criminal has a broad range of applications, such as monitoring gang activities, fraud detection, and improving performance of viral marketing . In this...Malik, Nomllllized cuts and image segmentation . Pattern Analysis and Machine Intelligence, IEEE Transactions on, 2000. 22(8): p. 888-905. [8] Wu

  16. Characterization of the Dilute Ising Antiferromagnet

    Energy Technology Data Exchange (ETDEWEB)

    Wiener, T.


    A spin glass is a magnetic ground state in which ferromagnetic and antiferromagnetic exchange interactions compete, thereby creating frustration and a multidegenerate state with no long range order. An Ising system is a system where the spins are constrained to lie parallel or antiparallel to a primary axis. There has been much theoretical interest in the past ten years in the effects of applying a magnetic field transverse to the primary axis in an Ising spin glass at low temperatures and thus study phase transitions at the T=0 limit. The focus of this study is to search for and characterize a new Ising spin glass system. This is accomplished by site diluting yttrium for terbium in the crystalline material TbNi{sub 2}Ge{sub 2}. The first part of this work gives a brief overview of the physics of rare earth magnetism and an overview of experimental characteristics of spin glasses. This is followed by the methodology used to manufacture the large single crystals used in this study, as well as the measurement techniques used. Next, a summary of the results of magnetic measurements on across the dilution series from pure terbium to pure yttrium is presented. This is followed by detailed measurements on particular dilutions which demonstrate spin glass behavior. Pure TbNi{sub 2}Ge{sub 2} is an Ising antiferromagnet with a several distinct metamagnetic states below 17 K. As the terbium is alloyed with yttrium, these magnetic states are weakened in a consistent manner, as is seen in measurements of the transition temperatures and analysis of Curie-Weiss behavior at high temperature. At low concentrations of terbium, below 35%, long range order is no longer present and a spin-glass-like state emerges. This state is studied through various measurements, dc and ac susceptibility, resistivity, and specific heat. This magnetic behavior was then compared to that of other well characterized spin glasses. It is concluded that there is a region of concentration s for which a spin

  17. Characterization of the Dilute Ising Antiferromagnet

    Energy Technology Data Exchange (ETDEWEB)

    Wiener, Timothy [Iowa State Univ., Ames, IA (United States)


    A spin glass is a magnetic ground state in which ferromagnetic and antiferromagnetic exchange interactions compete, thereby creating frustration and a multidegenerate state with no long range order. An Ising system is a system where the spins are constrained to lie parallel or antiparallel to a primary axis. There has been much theoretical interest in the past ten years in the effects of applying a magnetic field transverse to the primary axis in an Ising spin glass at low temperatures and thus study phase transitions at the T=0 limit. The focus of this study is to search for and characterize a new Ising spin glass system. This is accomplished by site diluting yttrium for terbium in the crystalline material TbNi2Ge2. The first part of this work gives a brief overview of the physics of rare earth magnetism and an overview of experimental characteristics of spin glasses. This is followed by the methodology used to manufacture the large single crystals used in this study, as well as the measurement techniques used. Next, a summary of the results of magnetic measurements on across the dilution series from pure terbium to pure yttrium is presented. This is followed by detailed measurements on particular dilutions which demonstrate spin glass behavior. Pure TbNi2Ge2 is an Ising antiferromagnet with a several distinct metamagnetic states below 17 K. As the terbium is alloyed with yttrium, these magnetic states are weakened in a consistent manner, as is seen in measurements of the transition temperatures and analysis of Curie-Weiss behavior at high temperature. At low concentrations of terbium, below 35%, long range order is no longer present and a spin-glass-like state emerges. This state is studied through various measurements, dc and ac susceptibility, resistivity, and specific heat. This magnetic behavior was then compared to that of other well characterized spin glasses. It is concluded that there is a region of

  18. DNA extraction protocol for biological ingredient analysis of Liuwei Dihuang Wan. (United States)

    Cheng, Xinwei; Chen, Xiaohua; Su, Xiaoquan; Zhao, Huanxin; Han, Maozhen; Bo, Cunpei; Xu, Jian; Bai, Hong; Ning, Kang


    Traditional Chinese medicine (TCM) preparations are widely used for healthcare and clinical practice. So far, the methods commonly used for quality evaluation of TCM preparations mainly focused on chemical ingredients. The biological ingredient analysis of TCM preparations is also important because TCM preparations usually contain both plant and animal ingredients, which often include some mis-identified herbal materials, adulterants or even some biological contaminants. For biological ingredient analysis, the efficiency of DNA extraction is an important factor which might affect the accuracy and reliability of identification. The component complexity in TCM preparations is high, and DNA might be destroyed or degraded in different degrees after a series of processing procedures. Therefore, it is necessary to establish an effective protocol for DNA extraction from TCM preparations. In this study, we chose a classical TCM preparation, Liuwei Dihuang Wan (LDW), as an example to develop a TCM-specific DNA extraction method. An optimized cetyl trimethyl ammonium bromide (CTAB) method (TCM-CTAB) and three commonly-used extraction kits were tested for extraction of DNA from LDW samples. Experimental results indicated that DNA with the highest purity and concentration was obtained by using TCM-CTAB. To further evaluate the different extraction methods, amplification of the second internal transcribed spacer (ITS2) and the chloroplast genome trnL intron was carried out. The results have shown that PCR amplification was successful only with template of DNA extracted by using TCM-CTAB. Moreover, we performed high-throughput 454 sequencing using DNA extracted by TCM-CTAB. Data analysis showed that 3-4 out of 6 prescribed species were detected from LDW samples, while up to 5 contaminating species were detected, suggesting TCM-CTAB method could facilitate follow-up DNA-based examination of TCM preparations. Copyright © 2014. Production and hosting by Elsevier Ltd.

  19. DNA Extraction Protocol for Biological Ingredient Analysis of Liuwei Dihuang Wan

    Institute of Scientific and Technical Information of China (English)

    Xinwei Cheng; Xiaohua Chen; Xiaoquan Su; Huanxin Zhao; Maozhen Han; Cunpei Bo; Jian Xu; Hong Bai; Kang Ning


    Traditional Chinese medicine (TCM) preparations are widely used for healthcare and clinical practice. So far, the methods commonly used for quality evaluation of TCM preparations mainly focused on chemical ingredients. The biological ingredient analysis of TCM preparations is also important because TCM preparations usually contain both plant and animal ingredients, which often include some mis-identified herbal materials, adulterants or even some biological con-taminants. For biological ingredient analysis, the efficiency of DNA extraction is an important fac-tor which might affect the accuracy and reliability of identification. The component complexity in TCM preparations is high, and DNA might be destroyed or degraded in different degrees after a series of processing procedures. Therefore, it is necessary to establish an effective protocol for DNA extraction from TCM preparations. In this study, we chose a classical TCM preparation, Liuwei Dihuang Wan (LDW), as an example to develop a TCM-specific DNA extraction method. An optimized cetyl trimethyl ammonium bromide (CTAB) method (TCM-CTAB) and three com-monly-used extraction kits were tested for extraction of DNA from LDW samples. Experimental results indicated that DNA with the highest purity and concentration was obtained by using TCM-CTAB. To further evaluate the different extraction methods, amplification of the second internal transcribed spacer (ITS2) and the chloroplast genome trnL intron was carried out.The results have shown that PCR amplification was successful only with template of DNA extracted by using TCM-CTAB. Moreover, we performed high-throughput 454 sequencing using DNA extracted by TCM-CTAB. Data analysis showed that 3-4 out of 6 prescribed species were detected from LDW samples, while up to 5 contaminating species were detected, suggesting TCM-CTAB method could facilitate follow-up DNA-based examination of TCM preparations.

  20. Multi-Scale Analysis Based Curve Feature Extraction in Reverse Engineering

    Institute of Scientific and Technical Information of China (English)

    YANG Hongjuan; ZHOU Yiqi; CHEN Chengjun; ZHAO Zhengxu


    A sectional curve feature extraction algorithm based on multi-scale analysis is proposed for reverse engineering. The algorithm consists of two parts: feature segmentation and feature classification. In the first part, curvature scale space is applied to multi-scale analysis and original feature detection. To obtain the primary and secondary curve primitives, feature fusion is realized by multi-scale feature detection information transmission. In the second part: projection height function is presented based on the area of quadrilateral, which improved criterions of sectional curve feature classification. Results of synthetic curves and practical scanned sectional curves are given to illustrate the efficiency of the proposed algorithm on feature extraction. The consistence between feature extraction based on multi-scale curvature analysis and curve primitives is verified.

  1. Liquid chromatography-mass spectrometry and chemometric analysis of Ricinus communis extracts for cultivar identification. (United States)

    Ovenden, Simon P B; Pigott, Eloise J; Rochfort, Simone; Bourne, David J


    Seeds of Ricinus communis contain the toxic protein ricin, a 64 kD heterodimeric type II ribosome-inactivating protein that has been used in several high-profile poisoning incidents. The ability to determine which cultivar the toxin was isolated from via an LC-MS method would be of significant use to law enforcement and forensic agencies. To analyse via LC-MS and chemometrics (principal components analysis (PCA), orthogonal partial-least-squares discriminant analysis (OPLS-DA)) extracts of R. communis to identify compounds specific to a particular cultivar. Seeds from eight specimens of six cultivars of R. communis ('carmencita', 'dehradun', 'gibsonii', 'impala', 'sanguineus' and 'zanzibariensis') were extracted using a standard methodology. These extracts were analysed by LC-MS then subjected to chemometric analysis (PCA and OPLS-DA). Identified compounds of importance were subjected to high-resolution Fourier transform (HRFT) MS and MS/MS to elucidate their structures. This analysis identified 17 ions as potential cultivar determinators. Through accurate mass measurement and MS/MS, molecular formulae for 13 ions were determined, including two known and 11 new peptides. Unique ions in extracts of 'carmencita', 'dehradun', 'gibsonii', 'impala' and 'zanzibariensis' were identified that would allow an individual cultivar to be distinguished from other cultivars in this study. Although 'sanguineus' extracts contained no unique compounds, a unique LC-MS profile would allow for cultivar assignment. Copyright © 2014 John Wiley & Sons, Ltd.

  2. Development of a routine analysis of 4-mercapto-4-methylpentan-2-one in wine by stable isotope dilution assay and mass tandem spectrometry. (United States)

    Dagan, Laurent; Reillon, Florence; Roland, Aurélie; Schneider, Rémi


    The 4-mercapto-4-methylpentan-2-one (4MMP) is a key aroma compound in wines, especially in Sauvignon Blanc ones. Its accurate quantification is quite difficult due to its traces levels and its reactivity in wine conferred by the thiol function. In this paper, we proposed a new method for its quantification in wine without any sample preparation, based on automated derivatization procedure by methoximation and SIDA-SPME-GC-MS/MS analysis. The derivatization procedure was adapted from a previously published method in order to decrease the amount of reagents and the volume of wine (only 3mL are required). The use of SPME and the detection conditions have also been optimized to reach the best sensitivity as possible. The method was then validated according to the International Organization of Vine and Wine recommendations and exhibited excellent performances. Indeed, this method allowed us to quantify the 4MMP in wine at traces levels (LOD=0.19 ng L(-1)) with reproducible results (RSD<15%) and a very good accuracy (recovery=102%). Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Academic vocabulary in learner writing from extraction to analysis

    CERN Document Server

    Paquot, Magali


    Academic vocabulary is in fashion, as witnessed by the increasing number of books published on the topic. In the first part of this book, Magali Paquot scrutinizes the concept of academic vocabulary and proposes a corpus-driven procedure based on the criteria of keyness, range and evenness of distribution to select academic words that could be part of a common-core academic vocabulary syllabus. In the second part, the author offers a thorough analysis of academic vocabulary in the International Corpus of Learner English (ICLE) and describes the factors that account for learners difficulties in

  4. Analysis of Usnea fasciata crude extracts with antineoplastic activity. (United States)

    Periera, E C; Nascimento, S C; Lima, R C; Silva, N H; Oliveira, A F; Bandeira, E; Boitard, M; Beriel, H; Vicente, C; Legaz, M E


    Different fractions, isolated from the lichen Usnea fasciata, were analyzed by PC, TLC, and RP-HPLC. Analysis of the organic phases, mainly containing phenolics, revealed that usnic acid is the main product from secondary metabolites, whereas the polysaccharides isolichenin and raffinose are the most abundant water-soluble carbohydrates. Fractions containing usnic acid, as well as those containing isolichenin, showed moderate activity against sarcoma 180 and Ehrlich tumor cells. High antitumoral activity, near 90% inhibition, was found associated with the fraction containing raffinose.

  5. Comparison of DNA extraction methods in analysis of salivary bacterial communities. (United States)

    Lazarevic, Vladimir; Gaïa, Nadia; Girard, Myriam; François, Patrice; Schrenzel, Jacques


    Culture-independent high-throughput sequencing-based methods are widely used to study bacterial communities. Although these approaches are superior to traditional culture-based methods, they introduce bias at the experimental and bioinformatics levels. We assessed the diversity of the human salivary microbiome by pyrosequencing of the 16S rDNA V1-3 amplicons using metagenomic DNA extracted by two different protocols: a simple proteinase K digestion without a subsequent DNA clean-up step, and a bead-beating mechanical lysis protocol followed by column DNA purification. A high degree of congruence was found between the two extraction methods, most notably in regard to the microbial community composition. The results showed that for a given bioinformatics pipeline, all the taxa with an average proportion >0.12% in samples processed using one extraction method were also detected in samples extracted using the other method. The same taxa tended to be abundant and frequent for both extraction methods. The relative abundance of sequence reads assigned to the phyla Actinobacteria, Spirochaetes, TM7, Synergistetes, and Tenericutes was significantly higher in the mechanically-treated samples than in the enzymatically-treated samples, whereas the phylum Firmicutes showed the opposite pattern. No significant differences in diversity indices were found between the extraction methods, although the mechanical lysis method revealed higher operational taxonomic unit richness. Differences between the extraction procedures outweighed the variations due to the bioinformatics analysis pipelines used.

  6. Comparison of DNA extraction methods in analysis of salivary bacterial communities.

    Directory of Open Access Journals (Sweden)

    Vladimir Lazarevic

    Full Text Available Culture-independent high-throughput sequencing-based methods are widely used to study bacterial communities. Although these approaches are superior to traditional culture-based methods, they introduce bias at the experimental and bioinformatics levels. We assessed the diversity of the human salivary microbiome by pyrosequencing of the 16S rDNA V1-3 amplicons using metagenomic DNA extracted by two different protocols: a simple proteinase K digestion without a subsequent DNA clean-up step, and a bead-beating mechanical lysis protocol followed by column DNA purification. A high degree of congruence was found between the two extraction methods, most notably in regard to the microbial community composition. The results showed that for a given bioinformatics pipeline, all the taxa with an average proportion >0.12% in samples processed using one extraction method were also detected in samples extracted using the other method. The same taxa tended to be abundant and frequent for both extraction methods. The relative abundance of sequence reads assigned to the phyla Actinobacteria, Spirochaetes, TM7, Synergistetes, and Tenericutes was significantly higher in the mechanically-treated samples than in the enzymatically-treated samples, whereas the phylum Firmicutes showed the opposite pattern. No significant differences in diversity indices were found between the extraction methods, although the mechanical lysis method revealed higher operational taxonomic unit richness. Differences between the extraction procedures outweighed the variations due to the bioinformatics analysis pipelines used.

  7. A Comparative Analysis of the 'Green' Techniques Applied for Polyphenols Extraction from Bioresources. (United States)

    Talmaciu, Adina Iulia; Volf, Irina; Popa, Valentin I


    From all the valuable biomass extractives, polyphenols are a widespread group of secondary metabolites found in all plants, representing the most desirable phytochemicals due to their potential to be used as additives in food industry, cosmetics, medicine, and others fields. At present, there is an increased interest to recover them from plant of spontaneous flora, cultivated plant, and wastes resulted in agricultural and food industry. That is why many efforts have been made to provide a highly sensitive, efficiently, and eco-friendly methods, for the extraction of polyphenols, according to the green chemistry and sustainable development concepts. Many extraction procedures are known with advantages and disadvantages. From these reasons, the aim of this article is to provide a comparative analysis regarding technical and economical aspects related to the most innovative extraction techniques studied in the last time: microwave-assisted extraction (MAE), supercritical fluid extraction (SFE), and ultrasound-assisted extraction (UAE). Copyright © 2015 Verlag Helvetica Chimica Acta AG, Zürich.

  8. Determination of terpenoid content in pine by organic solvent extraction and fast-GC analysis

    Directory of Open Access Journals (Sweden)

    Anne Elizabeth Harman-Ware


    Full Text Available Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts from the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β- pinene, camphene and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene and α-bisabolene. Diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic and neoabietic acids.

  9. Development and validation of an extraction method for the analysis of perfluoroalkyl substances in human hair. (United States)

    Kim, Da-Hye; Oh, Jeong-Eun


    Human hair has many advantages as a non-invasive sample; however, analytical methods for detecting perfluoroalkyl substances (PFASs) in human hair are still in the development stage. Therefore, the aim of this study was to develop and validate a method for monitoring 11 PFASs in human hair. Solid-phase extraction (SPE), ion-pairing extraction (IPE), a combined method (SPE+IPE) and solvent extraction with ENVI-carb clean-up were compared to develop an optimal extraction method using two types of hair sample (powder and piece forms). Analysis of PFASs was performed using liquid chromatography and tandem mass spectrometry. Among the four different extraction procedures, the SPE method using powdered hair showed the best extraction efficiency and recoveries ranged from 85.8 to 102%. The method detection limits for the SPE method were 0.114-0.796 ng/g and good precision (below 10%) and accuracy (66.4-110%) were obtained. In light of these results, SPE is considered the optimal method for PFAS extraction from hair. It was also successfully used to detect PFASs in human hair samples.


    Directory of Open Access Journals (Sweden)

    Kinjal Shah


    Full Text Available The incessant and vital need to discover new antimicrobial compounds with diverse chemical structures and novel mode of action is stimulated by the increasing failure of chemotherapeutics and expanded antibiotic resistance exhibited by pathogenic agents. In the present research work, antimicrobial activity of few plant extracts and ayurvedic samples were screened against bacteria. Phytochemical analysis of active plant extracts showed the presence of triterpenes, glycosides and flavonoids. Both aqueous and acetone extracts of Holoptelia integrifolia leaf and Barringtonia acutangula flower; and methanolic extract of Glycyrrhiza glabra and Meera powder exhibited activity against S. aureus. Aqueous mortar pestle and soxhlet extracts of B. acutangula flower exhibited activity against both P. aeruginosa and E. coli. Further, the ability to adhere and build biofilm was assessed in few biofilm formers at sub-MIC concentrations using the Microtiter plate assay and the Coverslip assay. Aqueous soxhlet and mortar pestle extract of B. acutangula flower and acetone overnight extract of H. integrifolia leaf exhibited antibiofilm activity against these organisms.

  11. Turbulence of Dilute Polymer Solution

    CERN Document Server

    Xi, Heng-Dong; Xu, Haitao


    In fully developed three dimensional fluid turbulence the fluctuating energy is supplied at large scales, cascades through intermediate scales, and dissipates at small scales. It is the hallmark of turbulence that for intermediate scales, in the so called inertial range, the average energy flux is constant and independent of viscosity [1-3]. One very important question is how this range is altered, when an additional agent that can also transport energy is added to the fluid. Long-chain polymers dissolved at very small concentrations in the fluid are such an agent [4,5]. Based on prior work by de Gennes and Tabor [6,7] we introduce a theory that balances the energy flux through the turbulent cascade with that of the energy flux into the elastic degrees of freedom of the dilute long-chain polymer solution. We propose a refined elastic length scale, $r_\\varepsilon$, which describes the effect of polymer elasticity on the turbulence energy cascade. Our experimental results agree excellently with this new energy ...

  12. 基于差分吸收激光雷达的一种新的对流层臭氧浓度反演算法%Butanol Extraction Combined with Dilute Hydrochloric Acid Dissolution-Atomic Fluorescence Spectrometric Method for Indirect Determination of Molybdenum in Chinese Herbal Medicine

    Institute of Scientific and Technical Information of China (English)

    范广强; 刘建国; 刘文清; 陆亦怀; 张天舒; 董云升; 赵雪松


    A method for indirectly determining the molybdenum in Chinese herbal medicine by butanol extraction and dilute hydrochloric acid dissolution was established for atomic fluorescence spectrometry. The molybdoarsenate heteropoly acid, formed in the presence of As( V) and ammonium molybdate in 0. 3 mol · L-1 sulphuric acid medium, was separated and enriched in the organic solvent, then the evaporation of organic reagent was implemented and the left residue was dissolved in dilute hydrochloric acid in which the arsenic content was determined on behalf of molybdenum. In the optimum experimental conditions, molybdenum content in 0~15 μg · L-1 range depicts a good linear relationship, the detection limit and relative standard deviation of 0. 44 μg · L-1 and 1.1% were obtained, respectively. Spiked Chinese herbal medicine samples were determined with the proposed method, and recoveries of 95. 6%—101. 3% were achieved.%差分吸收激光雷达探测对流层臭氧浓度时,气溶胶的干扰会造成较大的误差.提出了一种算法,该算法能够同时反演得到对流层臭氧浓度和气溶胶消光系数,减少气溶胶对反演结果的影响.使用实验数据,分析计算了气溶胶雷达比,气溶胶波长指数、标定点气溶胶后向散射比各种变化参数对反演结果的误差.结果表明,1km以下,各种变化参数造成的反演误差小于8%,1km以上臭氧浓度误差主要来源于信号和背景噪声,各种参数反演误差小于3%.最后给出了利用该算法得到对流层臭氧浓度和气溶胶的消光系数垂直廓线,并和传统的双波长差分算法反演结果作了比较分析.实验结果表明该算法是可行的,该算法可以减少气溶胶对差分吸收激光雷达测量结果引起的误差.

  13. RFI detection by automated feature extraction and statistical analysis (United States)

    Winkel, B.; Kerp, J.; Stanko, S.


    In this paper we present an interference detection toolbox consisting of a high dynamic range Digital Fast-Fourier-Transform spectrometer (DFFT, based on FPGA-technology) and data analysis software for automated radio frequency interference (RFI) detection. The DFFT spectrometer allows high speed data storage of spectra on time scales of less than a second. The high dynamic range of the device assures constant calibration even during extremely powerful RFI events. The software uses an algorithm which performs a two-dimensional baseline fit in the time-frequency domain, searching automatically for RFI signals superposed on the spectral data. We demonstrate, that the software operates successfully on computer-generated RFI data as well as on real DFFT data recorded at the Effelsberg 100-m telescope. At 21-cm wavelength RFI signals can be identified down to the 4σ_rms level. A statistical analysis of all RFI events detected in our observational data revealed that: (1) mean signal strength is comparable to the astronomical line emission of the Milky Way, (2) interferences are polarised, (3) electronic devices in the neighbourhood of the telescope contribute significantly to the RFI radiation. We also show that the radiometer equation is no longer fulfilled in presence of RFI signals.

  14. RFI detection by automated feature extraction and statistical analysis

    CERN Document Server

    Winkel, B; Stanko, S; Winkel, Benjamin; Kerp, Juergen; Stanko, Stephan


    In this paper we present an interference detection toolbox consisting of a high dynamic range Digital Fast-Fourier-Transform spectrometer (DFFT, based on FPGA-technology) and data analysis software for automated radio frequency interference (RFI) detection. The DFFT spectrometer allows high speed data storage of spectra on time scales of less than a second. The high dynamic range of the device assures constant calibration even during extremely powerful RFI events. The software uses an algorithm which performs a two-dimensional baseline fit in the time-frequency domain, searching automatically for RFI signals superposed on the spectral data. We demonstrate, that the software operates successfully on computer-generated RFI data as well as on real DFFT data recorded at the Effelsberg 100-m telescope. At 21-cm wavelength RFI signals can be identified down to the 4-sigma level. A statistical analysis of all RFI events detected in our observational data revealed that: (1) mean signal strength is comparable to the a...

  15. Automatic knowledge extraction in sequencing analysis with multiagent system and grid computing. (United States)

    González, Roberto; Zato, Carolina; Benito, Rocío; Bajo, Javier; Hernández, Jesús M; De Paz, Juan F; Vera, Vicente; Corchado, Juan M


    Advances in bioinformatics have contributed towards a significant increase in available information. Information analysis requires the use of distributed computing systems to best engage the process of data analysis. This study proposes a multiagent system that incorporates grid technology to facilitate distributed data analysis by dynamically incorporating the roles associated to each specific case study. The system was applied to genetic sequencing data to extract relevant information about insertions, deletions or polymorphisms.

  16. Innovative analysis of 3-mercaptohexan-1-ol, 3-mercaptohexylacetate and their corresponding disulfides in wine by stable isotope dilution assay and nano-liquid chromatography tandem mass spectrometry. (United States)

    Roland, Aurélie; Delpech, Stéphane; Dagan, Laurent; Ducasse, Marie-Agnès; Cavelier, Florine; Schneider, Rémi


    Both 3-mercaptohexan-1-ol (3MH) and 3-mercaptohexyl acetate (3MHA) were largely studied for the last 20 years due to their pleasant olfactory notes conferred to wine. Until now, many analytical methods focused only on the free forms of both 3MH and 3MHA in wine that provided partial information in the wine aroma evolution. Our study proposes new analytical measurements which allow quantification of both free and disulfide forms of 3MH and 3MHA to better understand the redox phenomenon occurring in wines and further, to orientate wine aroma evolution. Free thiols were analyzed by an original method based on maleimide derivatization allowing in-situ disulfide reduction followed by SIDA-LC-MS/MS analyses exhibiting excellent performances. Indeed, the accuracy ranged from 95 to 110% in three different wine matrices and the repeatability and intermediate reproducibility were inferior to 15% (RSD measurements). Our method exhibited very low limits of detection, which are below to 0.5ng/L and inferior to the perception thresholds of both compounds. Then, this method was applied to three different wines exposed to several oxidative conditions. On the one hand, it was demonstrated that copper sulfate treatment firstly destroyed the total amount of free 3MH to the benefit of thioether and disulfides compounds, with proportions that could be slightly modified by glutathione addition. On the other hand, oxygenation of wines resulted in partial free 3MH destruction to the benefit of thioether compounds. We proposed for the first time an innovative analysis that gives a complete picture of wine aroma, which can be really useful to winemakers to manage wine aroma evolution and to take advantage of the disulfide reservoir. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. GC-MS analysis of bioactive compounds in the methanol extract of Clerodendrum viscosum leaves

    Directory of Open Access Journals (Sweden)

    Pritipadma Panda


    Full Text Available Background: Clerodendrum viscosum is commonly found in India and Bangladesh. Previously, various parts of this plant were reported for treatment of different types of diseases and there was no report on GC-Ms analysis. Objective: To analyze and characterize the phytochemical compounds of methanol extract of Clerodendrum viscosum using GC-MS. Materials and Methods: The preliminary phytochemical screening of methanol extract was carried out according to standard procedures described in WHO guidelines. Various bioactive compounds of the extract were determined by GC-MS technique. Results: The presence of steroids, triterpenoids, alkaloids, saponins, flavonoids, tannins and carbohydrate was found on phytochemical screening of methanol extract of the leaves. The GC-MS analysis showed 16 peaks of different phytoconstituents namely acetamide,N,N-carbonylbis-, 4-Pyranone,2,3-dihydro-, alpha-D-Galactofuranoside, methyl 2,3,5,6-tetra-O-methyl-, Glycerin, Xylitol, N,N-Dimethylglycine, 4H-Pyran-4-one,2,3-dihydro-3, 5-dihydroxy-6-methyl-, Benzofuran,2,3-dihydro-, 5-Hydroxymethylfurfural, 2(1HPyrimidinone,1-methyl-, 2,4-Dihydroxy-5,6-dimethylpyrimidine, 3-Deoxy-d-mannoic lactone, 1,3-Methylene-d-arabitol, Orcinol, n-Hexadecanoic acid and Phenol,4,4′-(1-methyl ethylidene bis etc. Conclusion: The bioactive compounds present in the methanol extract of Clerodendrum viscosum suggest the application of this extract for the treatment of various diseases by the aborigine tribes.

  18. Capillary electrophoretic analysis of flavonoids in single-styled hawthorn (Crataegus monogyna Jacq.) ethanolic extracts. (United States)

    Urbonaviciūte, A; Jakstas, V; Kornysova, O; Janulis, V; Maruska, A


    Flavonoids are an important group of natural compounds, which can prevent coronary heart disease and have antioxidant properties. Hawthorn is a well known and widely used medicinal plant due to its cardiotonic activity. Previous studies refer mostly to the HPLC analysis of the flavonoids: vitexin, quercetin, hyperoside, oligomeric procyanidins, which appear to be primarily responsible for the cardiac action of the plant. Aqueous ethanolic extracts of single-styled hawthorn (Crataegus monogyna Jacq., f.: Rosaceae Juss.) leaves and sprouts were analyzed by means of capillary zone electrophoresis (CZE). Influence of vegetation period on the extract qualitative composition and flavonoids quantities was evaluated. Sample preparation by extraction using different concentration of aqueous ethanol (40-96%, v/v) and the influence of extractant composition on the recovery of flavonoids are discussed in detail. The results obtained using CZE are compared to the results of spectrophotometric and HPLC analysis of the extracts. The effect of storage conditions of extracts (solar irradiation, temperature and duration) on degradation of flavonoids was investigated.

  19. Knee cartilage extraction and bone-cartilage interface analysis from 3D MRI data sets (United States)

    Tamez-Pena, Jose G.; Barbu-McInnis, Monica; Totterman, Saara


    This works presents a robust methodology for the analysis of the knee joint cartilage and the knee bone-cartilage interface from fused MRI sets. The proposed approach starts by fusing a set of two 3D MR images the knee. Although the proposed method is not pulse sequence dependent, the first sequence should be programmed to achieve good contrast between bone and cartilage. The recommended second pulse sequence is one that maximizes the contrast between cartilage and surrounding soft tissues. Once both pulse sequences are fused, the proposed bone-cartilage analysis is done in four major steps. First, an unsupervised segmentation algorithm is used to extract the femur, the tibia, and the patella. Second, a knowledge based feature extraction algorithm is used to extract the femoral, tibia and patellar cartilages. Third, a trained user corrects cartilage miss-classifications done by the automated extracted cartilage. Finally, the final segmentation is the revisited using an unsupervised MAP voxel relaxation algorithm. This final segmentation has the property that includes the extracted bone tissue as well as all the cartilage tissue. This is an improvement over previous approaches where only the cartilage was segmented. Furthermore, this approach yields very reproducible segmentation results in a set of scan-rescan experiments. When these segmentations were coupled with a partial volume compensated surface extraction algorithm the volume, area, thickness measurements shows precisions around 2.6%

  20. Region of interest extraction based on multiscale visual saliency analysis for remote sensing images (United States)

    Zhang, Yinggang; Zhang, Libao; Yu, Xianchuan


    Region of interest (ROI) extraction is an important component of remote sensing image processing. However, traditional ROI extraction methods are usually prior knowledge-based and depend on classification, segmentation, and a global searching solution, which are time-consuming and computationally complex. We propose a more efficient ROI extraction model for remote sensing images based on multiscale visual saliency analysis (MVS), implemented in the CIE L*a*b* color space, which is similar to visual perception of the human eye. We first extract the intensity, orientation, and color feature of the image using different methods: the visual attention mechanism is used to eliminate the intensity feature using a difference of Gaussian template; the integer wavelet transform is used to extract the orientation feature; and color information content analysis is used to obtain the color feature. Then, a new feature-competition method is proposed that addresses the different contributions of each feature map to calculate the weight of each feature image for combining them into the final saliency map. Qualitative and quantitative experimental results of the MVS model as compared with those of other models show that it is more effective and provides more accurate ROI extraction results with fewer holes inside the ROI.

  1. Feature Extraction Using Supervised Independent Component Analysis by Maximizing Class Distance (United States)

    Sakaguchi, Yoshinori; Ozawa, Seiichi; Kotani, Manabu

    Recently, Independent Component Analysis (ICA) has been applied to not only problems of blind signal separation, but also feature extraction of patterns. However, the effectiveness of pattern features extracted by conventional ICA algorithms depends on pattern sets; that is, how patterns are distributed in the feature space. As one of the reasons, we have pointed out that ICA features are obtained by increasing only their independence even if the class information is available. In this context, we can expect that more high-performance features can be obtained by introducing the class information into conventional ICA algorithms. In this paper, we propose a supervised ICA (SICA) that maximizes Mahalanobis distance between features of different classes as well as maximize their independence. In the first experiment, two-dimensional artificial data are applied to the proposed SICA algorithm to see how maximizing Mahalanobis distance works well in the feature extraction. As a result, we demonstrate that the proposed SICA algorithm gives good features with high separability as compared with principal component analysis and a conventional ICA. In the second experiment, the recognition performance of features extracted by the proposed SICA is evaluated using the three data sets of UCI Machine Learning Repository. From the results, we show that the better recognition accuracy is obtained using our proposed SICA. Furthermore, we show that pattern features extracted by SICA are better than those extracted by only maximizing the Mahalanobis distance.

  2. Storm Sewage Dilution in Smaller Streams

    DEFF Research Database (Denmark)

    Larsen, Torben; Vestergaard, Kristian


    A numerical model has been used to show how dilution in smaller streams can be effected by unsteady hydraulic conditions caused by a storm sewage overflow.......A numerical model has been used to show how dilution in smaller streams can be effected by unsteady hydraulic conditions caused by a storm sewage overflow....

  3. [Fetal electrocardiogram extraction based on independent component analysis and quantum particle swarm optimizer algorithm]. (United States)

    Du, Yanqin; Huang, Hua


    Fetal electrocardiogram (FECG) is an objective index of the activities of fetal cardiac electrophysiology. The acquired FECG is interfered by maternal electrocardiogram (MECG). How to extract the fetus ECG quickly and effectively has become an important research topic. During the non-invasive FECG extraction algorithms, independent component analysis(ICA) algorithm is considered as the best method, but the existing algorithms of obtaining the decomposition of the convergence properties of the matrix do not work effectively. Quantum particle swarm optimization (QPSO) is an intelligent optimization algorithm converging in the global. In order to extract the FECG signal effectively and quickly, we propose a method combining ICA and QPSO. The results show that this approach can extract the useful signal more clearly and accurately than other non-invasive methods.

  4. Tissue extraction of DNA and RNA and analysis by the polymerase chain reaction. (United States)

    Jackson, D P; Lewis, F A; Taylor, G R; Boylston, A W; Quirke, P


    Several DNA extraction techniques were quantitatively and qualitatively compared using both fresh and paraffin wax embedded tissue and their suitability investigated for providing DNA and RNA for the polymerase chain reaction (PCR). A one hour incubation with proteinase K was the most efficient DNA extraction procedure for fresh tissue. For paraffin wax embedded tissue a five day incubation with proteinase K was required to produce good yields of DNA. Incubation with sodium dodecyl sulphate produced very poor yields, while boiling produced 20% as much DNA as long enzyme digestion. DNA extracted by these methods was suitable for the PCR amplification of a single copy gene. Proteinase K digestion also produced considerable amounts of RNA which has previously been shown to be suitable for PCR analysis. A delay before fixation had no effect on the amount of DNA obtained while fixation in Carnoy's reagent results in a much better preservation of DNA than formalin fixation, allowing greater yields to be extracted.

  5. Analysis of Benzo[a]pyrene in Vegetable Oils Using Molecularly Imprinted Solid Phase Extraction (MISPE Coupled with Enzyme-Linked Immunosorbent Assay (ELISA

    Directory of Open Access Journals (Sweden)

    Michael Pschenitza


    Full Text Available This paper describes the development of a molecularly imprinted polymer-based solid phase extraction (MISPE method coupled with enzyme-linked immunosorbent assay (ELISA for determination of the PAH benzo[a]pyrene (B[a]P in vegetable oils. Different molecularly imprinted polymers (MIPs were prepared using non-covalent 4-vinylpyridine/divinylbenzene co-polymerization at different ratios and dichloromethane as porogen. Imprinting was done with a template mixture of phenanthrene and pyrene yielding a broad-specific polymer for PAHs with a maximum binding capacity (Q of ~32 μg B[a]P per 50 mg of polymer. The vegetable oil/n-hexane mixture (1:1, (v/v was pre-extracted with acetonitrile, the solvent evaporated, the residue reconstituted in n-hexane and subjected to MISPE. The successive washing with n-hexane and isopropanol revealed most suitable to remove lipid matrix constituents. After elution of bound PAHs from MISPE column with dichloromethane, the solvent was evaporated, the residue reconstituted with dimethyl sulfoxide and diluted 100-fold with methanol/water (10:90, (v/v for analysis of B[a]P equivalents with an ELISA. The B[a]P recovery rates in spiked vegetable oil samples of different fatty acid composition were determined between 63% and 114%. The presence of multiple PAHs in the oil sample, because of MIP selectivity and cross-reactivity of the ELISA, could yield overestimated B[a]P values.

  6. Automated Extraction of Archaeological Traces by a Modified Variance Analysis

    Directory of Open Access Journals (Sweden)

    Tiziana D'Orazio


    Full Text Available This paper considers the problem of detecting archaeological traces in digital aerial images by analyzing the pixel variance over regions around selected points. In order to decide if a point belongs to an archaeological trace or not, its surrounding regions are considered. The one-way ANalysis Of VAriance (ANOVA is applied several times to detect the differences among these regions; in particular the expected shape of the mark to be detected is used in each region. Furthermore, an effect size parameter is defined by comparing the statistics of these regions with the statistics of the entire population in order to measure how strongly the trace is appreciable. Experiments on synthetic and real images demonstrate the effectiveness of the proposed approach with respect to some state-of-the-art methodologies.

  7. Screening for Antibacterial and Antioxidant Activities and Phytochemical Analysis of Oroxylum indicum Fruit Extracts

    Directory of Open Access Journals (Sweden)

    Patchima Sithisarn


    Full Text Available Oroxylum indicum, which is called Pheka in Thai, is a traditional Thai plant in the Bignoniaceae family with various ethnomedical uses such as as an astringent, an anti-inflammatory agent, an anti-bronchitic agent, an anti-helminthic agent and an anti-microbial agent. The young fruits of this plant have also been consumed as vegetables. However, there has been no report concerning its antibacterial activities, especially activities related to clinically isolated pathogenic bacteria and the in vitro antioxidant effects of this plant. Therefore, the extracts from O. indicum fruits and seeds collected from different provinces in Thailand were prepared by decoction and maceration with ethanol and determined for their in vitro antibacterial effects on two clinically isolated bacteria, Streptococcus suis and Staphylococcus intermedius, using disc diffusion assay. Ethanol extracts from O. indicum fruits collected from Nakorn Pathom province at the concentration of 1000 mg/mL exhibited intermediate antibacterial activity against S. intermedius with an inhibition zone of 15.11 mm. Moreover, it promoted moderate inhibitory effects on S. suis with an inhibition zone of 14.39 mm. The extracts prepared by maceration with ethanol promoted higher antibacterial activities than those prepared with water. The ethanol extract from the seeds of this plant, purchased in Bangkok, showed stronger in vitro antioxidant activities than the other extracts, with an EC50 value of 26.33 µg/mL. Phytochemical analysis suggested that the seed ethanol extract contained the highest total phenolic and flavonoid contents (10.66 g% gallic acid equivalent and 7.16 g% quercetin equivalent, respectively by a significant amount. Thin layer chromatographic analysis of the extracts showed the chromatographic band that could correspond to a flavonoid baicalein. From the results, extracts from O. indicum fruits have an in vitro antioxidant effect, with antibacterial potential, on

  8. GC/GCMS analysis of the petroleum ether and dichloromethane extracts of Moringa oleifera roots

    Institute of Scientific and Technical Information of China (English)

    Shaheen Faizi; Saima Sumbul; Muhammed Ali Versiani; Rubeena Saleem; Aisha Sana; Hira Siddiqui


    Objective:To explore the phytochemical constituents from petroleum ether and dichloromethane extracts of Moringa oleifera (M. oleifera) roots using GC/GC-MS. Methods: A total of 5.11 kg fresh and undried crushed root of M. oleifera were cut into small pieces and extracted with petroleum ether and dichloromethane (20 L each) at room temperature for 2 d. The concentrated extracts were subjected to their GC-MS analysis. Results:The GC-MS analysis of the petroleum ether and dichloromethane extracts of M. oleifera roots, which showed promising biological activities, has resulted in the identification 102 compounds. These constituents belong to 15 classes of compounds including hydrocarbons, fatty acids, esters, alcohols, isothiocyanate, thiocyanate, pyrazine, aromatics, alkamides, cyanides, steroids, halocompounds, urea and N-hydroxyimine derivatives, unsaturated alkenamides, alkyne and indole. GC/GC-MS studies on petroleum ether extract of the roots revealed that it contained 39 compounds, belonging to nine classes. Cyclooctasulfur S8 has been isolated as a pure compound from the extract. The major compounds identified from petroleum ether extract were trans-13-docosene (37.9%), nonacosane (32.6%), cycloartenol (28.6%) nonadecanoic acid (13.9%) and cyclooctasulfur S8 (13.9%). Dichloromethane extract of the roots was composed of 63 compounds of which nasimizinol (58.8%) along with oleic acid (46.5%), N-benzyl-N-(7-cyanato heptanamide (38.3%), N-benzyl-N-(1-chlorononyl) amide (30.3%), bis [3-benzyl prop-2-ene]-1-one (19.5%) and N, N-dibenzyl-2-ene pent 1, 5-diamide (11.6%) were the main constituents. Conclusions:This study helps to predict the formula and structure of active molecules which can be used as drugs. This result also enhances the traditional usage of M. oleifera which possesses a number of bioactive compounds.

  9. Screening for Antibacterial and Antioxidant Activities and Phytochemical Analysis of Oroxylum indicum Fruit Extracts. (United States)

    Sithisarn, Patchima; Nantateerapong, Petcharat; Rojsanga, Piyanuch; Sithisarn, Pongtip


    Oroxylum indicum, which is called Pheka in Thai, is a traditional Thai plant in the Bignoniaceae family with various ethnomedical uses such as as an astringent, an anti-inflammatory agent, an anti-bronchitic agent, an anti-helminthic agent and an anti-microbial agent. The young fruits of this plant have also been consumed as vegetables. However, there has been no report concerning its antibacterial activities, especially activities related to clinically isolated pathogenic bacteria and the in vitro antioxidant effects of this plant. Therefore, the extracts from O. indicum fruits and seeds collected from different provinces in Thailand were prepared by decoction and maceration with ethanol and determined for their in vitro antibacterial effects on two clinically isolated bacteria, Streptococcus suis and Staphylococcus intermedius, using disc diffusion assay. Ethanol extracts from O. indicum fruits collected from Nakorn Pathom province at the concentration of 1000 mg/mL exhibited intermediate antibacterial activity against S. intermedius with an inhibition zone of 15.11 mm. Moreover, it promoted moderate inhibitory effects on S. suis with an inhibition zone of 14.39 mm. The extracts prepared by maceration with ethanol promoted higher antibacterial activities than those prepared with water. The ethanol extract from the seeds of this plant, purchased in Bangkok, showed stronger in vitro antioxidant activities than the other extracts, with an EC50 value of 26.33 µg/mL. Phytochemical analysis suggested that the seed ethanol extract contained the highest total phenolic and flavonoid contents (10.66 g% gallic acid equivalent and 7.16 g% quercetin equivalent, respectively) by a significant amount. Thin layer chromatographic analysis of the extracts showed the chromatographic band that could correspond to a flavonoid baicalein. From the results, extracts from O. indicum fruits have an in vitro antioxidant effect, with antibacterial potential, on clinically pathologic

  10. Use of solvent mixtures for total lipid extraction of Chlorella vulgaris and gas chromatography FAME analysis. (United States)

    Moradi-Kheibari, Narges; Ahmadzadeh, Hossein; Hosseini, Majid


    Lipid extraction is the bottleneck step for algae-based biodiesel production. Herein, 12 solvent mixture systems (mixtures of three non-polar and two polar organic solvents) were examined to evaluate their effects on the total lipid yield from Chlorella vulgaris (C. vulgaris). Moreover, the extraction yields of three solvent systems with maximum extraction efficiency of esterifiable lipids were determined by acidic transesterification and GC-FID analysis. Three solvent systems, which resulted in a higher extraction yield, were further subjected to fatty acid methyl ester (FAME) analysis. The total lipid extraction yields (based on dry biomass) were (38.57 ± 1.51), (25.33 ± 0.58), and (25.17 ± 1.14) %, for chloroform-methanol (1:2) (C1M2), hexane-methanol (1:2) (H1M2), and chloroform-methanol (2:1) (C2M1), respectively. The extraction efficiency of C1M2 was approximately 1.5 times higher than H1M2 and C2M1, whereas the FAME profile of extracted lipids by H1M2 and C1M2 were almost identical. Moreover, the esterifiable lipid extraction yields of (18.14 ± 2.60), (16.66 ± 0.35), and (13.22 ± 0.31) % (based on dry biomass) were obtained for C1M2, H1M2, and C2M1 solvent mixture systems, respectively. The biodiesel fuel properties produced from C. vulgaris were empirically predicted and compared to that of the EN 14214 and ASTM 6751 standard specifications.

  11. Improved Proteomic Analysis Following Trichloroacetic Acid Extraction of Bacillus anthracis Spore Proteins

    Energy Technology Data Exchange (ETDEWEB)

    Kaiser, Brooke LD; Wunschel, David S.; Sydor, Michael A.; Warner, Marvin G.; Wahl, Karen L.; Hutchison, Janine R.


    Proteomic analysis of bacterial samples provides valuable information about cellular responses and functions under different environmental pressures. Proteomic analysis is dependent upon efficient extraction of proteins from bacterial samples without introducing bias toward extraction of particular protein classes. While no single method can recover 100% of the bacterial proteins, selected protocols can improve overall protein isolation, peptide recovery, or enrich for certain classes of proteins. The method presented here is technically simple and does not require specialized equipment such as a mechanical disrupter. Our data reveal that for particularly challenging samples, such as B. anthracis Sterne spores, trichloroacetic acid extraction improved the number of proteins identified within a sample compared to bead beating (714 vs 660, respectively). Further, TCA extraction enriched for 103 known spore specific proteins whereas bead beating resulted in 49 unique proteins. Analysis of C. botulinum samples grown to 5 days, composed of vegetative biomass and spores, showed a similar trend with improved protein yields and identification using our method compared to bead beating. Interestingly, easily lysed samples, such as B. anthracis vegetative cells, were equally as effectively processed via TCA and bead beating, but TCA extraction remains the easiest and most cost effective option. As with all assays, supplemental methods such as implementation of an alternative preparation method may provide additional insight to the protein biology of the bacteria being studied.

  12. Information Extraction for System-Software Safety Analysis: Calendar Year 2008 Year-End Report (United States)

    Malin, Jane T.


    This annual report describes work to integrate a set of tools to support early model-based analysis of failures and hazards due to system-software interactions. The tools perform and assist analysts in the following tasks: 1) extract model parts from text for architecture and safety/hazard models; 2) combine the parts with library information to develop the models for visualization and analysis; 3) perform graph analysis and simulation to identify and evaluate possible paths from hazard sources to vulnerable entities and functions, in nominal and anomalous system-software configurations and scenarios; and 4) identify resulting candidate scenarios for software integration testing. There has been significant technical progress in model extraction from Orion program text sources, architecture model derivation (components and connections) and documentation of extraction sources. Models have been derived from Internal Interface Requirements Documents (IIRDs) and FMEA documents. Linguistic text processing is used to extract model parts and relationships, and the Aerospace Ontology also aids automated model development from the extracted information. Visualizations of these models assist analysts in requirements overview and in checking consistency and completeness.

  13. Data extraction for complex meta-analysis (DECiMAL) guide. (United States)

    Pedder, Hugo; Sarri, Grammati; Keeney, Edna; Nunes, Vanessa; Dias, Sofia


    As more complex meta-analytical techniques such as network and multivariate meta-analyses become increasingly common, further pressures are placed on reviewers to extract data in a systematic and consistent manner. Failing to do this appropriately wastes time, resources and jeopardises accuracy. This guide (data extraction for complex meta-analysis (DECiMAL)) suggests a number of points to consider when collecting data, primarily aimed at systematic reviewers preparing data for meta-analysis. Network meta-analysis (NMA), multiple outcomes analysis and analysis combining different types of data are considered in a manner that can be useful across a range of data collection programmes. The guide has been shown to be both easy to learn and useful in a small pilot study.

  14. Information extraction from topographic map using colour and shape analysis

    Indian Academy of Sciences (India)

    Nikam Gitanjali Ganpatrao; Jayanta Kumar Ghosh


    The work presented in this paper is related to symbols and toponym understanding with application to scanned Indian topographic maps. The proposed algorithm deals with colour layer separation of enhanced topographic map using kmeans colour segmentation followed by outline detection and chaining, respectively. Outline detection is performed through linear filtering using canny edge detector. Outline is then encoded in a Freeman way, the x-y offsets have been used to obtain a complex representation of outlines. Final matching of shapes is done by computing Fourier descriptors from the chain-codes; comparison of descriptors having same colour index is embedded in a normalized scalar product of descriptors. As this matching process is not rotation invariant (starting point selection), an interrelation function has been proposed to make the method shifting invariant. The recognition rates of symbols, letters and numbers are 84.68, 91.73 and 92.19%, respectively. The core contribution is dedicated to a shape analysis method based on contouring and Fourier descriptors. To improve recognition rate, obtaining most optimal segmentation solution for complex topographic map will be the future scope of work.

  15. Exhaustive extraction of peptides by electromembrane extraction

    DEFF Research Database (Denmark)

    Huang, Chuixiu; Gjelstad, Astrid; Pedersen-Bjergaard, Stig


    device. Mass transfer of peptides across the SLM was enhanced by complex formation with the negatively charged DEHP. The composition of the SLM and the extraction voltage were important factors influencing recoveries and current with the EME system. 1-nonanol diluted with 2-decanone (1:1 v/v) containing...

  16. Extraction of heavy metals characteristics of the 2011 Tohoku tsunami deposits using multiple classification analysis. (United States)

    Nakamura, Kengo; Kuwatani, Tatsu; Kawabe, Yoshishige; Komai, Takeshi


    Tsunami deposits accumulated on the Tohoku coastal area in Japan due to the impact of the Tohoku-oki earthquake. In the study reported in this paper, we applied principal component analysis (PCA) and cluster analysis (CA) to determine the concentrations of heavy metals in tsunami deposits that had been diluted with water or digested using 1 M HCl. The results suggest that the environmental risk is relatively low, evidenced by the following geometric mean concentrations: Pb, 16 mg kg(-1) and 0.003 ml L(-1); As, 1.8 mg kg(-1) and 0.004 ml L(-1); and Cd, 0.17 mg kg(-1) and 0.0001 ml L(-1). CA was performed after outliers were excluded using PCA. The analysis grouped the concentrations of heavy metals for leaching in water and acid. For the acid case, the first cluster contained Ni, Fe, Cd, Cu, Al, Cr, Zn, and Mn; while the second contained Pb, Sb, As, and Mo. For water, the first cluster contained Ni, Fe, Al, and Cr; and the second cluster contained Mo, Sb, As, Cu, Zn, Pb, and Mn. Statistical analysis revealed that the typical toxic elements, As, Pb, and Cd have steady correlations for acid leaching but are relatively sparse for water leaching. Pb and As from the tsunami deposits seemed to reveal a kind of redox elution mechanism using 1 M HCl.

  17. Phytochemical analysis and in vitro antioxidant acitivity of hydroalcoholic seed extract of Nymphaea nouchali Burm. f.

    Institute of Scientific and Technical Information of China (English)

    Mabel Parimala; Francis Gricilda Shoba


    Objective: To evaluate the phytochemical constituents and the antioxidant activity of hydroalcoholic extract of Nymphaea nouchali seed locally prescribed as a diet for diabetes mellitus.Methods:the plant was assessed against 1,1 diphenyl-2-picryl hydrazyl (DPPH), nitric oxide and lipid peroxidation using standard protocols. Total phenolics, flavonoids and tannins were also determined.Results:Phytochemical analysis revealed the presence of phenols, flavones, tannins, protein, The antioxidant and free radical scavenging activity of hydroalcoholic extract of reducing sugars, glycosides, saponins, alkaloids and steroids. The activities of plant extract against DPPH, nitric oxide and lipid peroxidation was concentration dependent with IC50 value of 42.82, 23.58 and 54.65 µg/mL respectively. The total antioxidant capacity was high with 577.73 mg vitamin E/g of the extract and showed a moderately high vitamin C content of 197.22 mg/g. The total tannin content of hydroalcoholic seed extract was high (195.84 GE/g), followed by phenolics (179.56 GE/g) and flavonoids (23.55 QE/g).Conclusion:Our findings provide evidence that the crude extract of Nymphaea nouchali is a potential source of natural antioxidants and this justifies its use in folkloric medicine.

  18. Ultrasound-assisted extraction, HPLC analysis, and antioxidant activity of polyphenols from unripe apple. (United States)

    Yue, Tianli; Shao, Dongyan; Yuan, Yahong; Wang, Zhouli; Qiang, Chunyan


    The polyphenols were extracted from the unripe apple assisted by a highly efficient and simple method of the ultrasound. Response surface methodology was used to investigate the effects of processing parameters, including ultrasound power, extraction time, temperature, and ethanol concentration on total polyphenols yield and polyphenols composition was analyzed by HPLC. Antioxidant activity of the polyphenols was evaluated as 2, 2-diphenyl-1-picrylhydracyl scavenging activity and inhibition activity of lipid peroxidation. The results showed that 10-100 times higher total polyphenols yield was obtained from the unripe apple than those from the reported apple pomace. The optimum extraction conditions were ultrasonic power of 519.39 W, extraction time of 30 min, extraction temperature 50°C, ethanol concentration of 50% gave the total polyphenols yield of 13.26 ± 0.56 mg GAE/g. HPLC analysis indicated that (-)-epicatechin, procyanidin B2, chlorogenic acid, and procyanidin B1 were the predominant polyphenols in unripe apple, which contributed to the higher antioxidant activity to 2, 2-diphenyl-1-picrylhydracyl of unripe apple polyphenols than other apple polyphenols. The extracted polyphenols had higher ability to inhibit lipid peroxidation than butylated hydroxy toluene, which demonstrated that the unripe apple polyphenols have the potential to be used as a substitute of some synthetic antioxidants.

  19. Antimicrobial Activity and Phytochemical Analysis of Morinda tinctoria Roxb. Leaf Extracts

    Institute of Scientific and Technical Information of China (English)

    K Deepti; PUmadevi; GVijayalakshmi; BVinod polarao


    Objective: The objective of the present work is to evaluate the presence of Phytochemical constituents and antimicrobial activity of different extracts of leaves of Morinda tinctoria Roxb. Methods: The serial exhaustive extraction was done with a series of solvents: Hexane, Chloroform, Ethylacetate and Methanol with increasing polarity using soxhlet apparatus. The Phytochemical analysis was done by using the standard procedures. Antimicrobial activity was evaluated by Agar well diffusion method against nine human pathogens. Results: The results revealed that the leaf extracts contain a broad spectrum of secondary metabolites: Alkaloids, Phytosterols, Flavonoids, Phenols and Triterpenes in major proportion. Methanol extract was shown to be more effective against all the organisms followed by Ethylacetate, Chloroform and Hexane extracts. Proteus vulgaris (24mm) was found to be most sensitive organism followed by Klebsiella pneumonia (21mm) and Enterococcus feacelis (21mm). Conclusions: The present study concludes that the different extracts of M. tinctoria leaves contain a broad spectrum of secondary metabolites and also exhibit antimicrobial activity against all the tested microorganisms. It can also be concluded that Morinda tinctoria plant can be exploited to discover the bioactive natural products that may serve as leads in the development of new pharmaceuticals.

  20. Region of interest extraction based on saliency detection and contrast analysis for remote sensing images (United States)

    Lv, Jing; Zhang, Libao; Wang, Shuang


    Region of Interest (ROI) extraction is an important component in remote sensing images processing, which is useful for further practical applications such as image compression, image fusion, image segmentation and image registration. Traditional ROI extraction methods are usually prior knowledge-based and depend on a global searching solution which are time consuming and computational complex. Saliency detection which is widely used for ROI extraction from natural scene images in these years can effectively solve the problem of high computation complexity in ROI extraction for remote sensing images as well as retain accuracy. In this paper, a new computational model is proposed to improve the accuracy of ROI extraction in remote sensing images. Considering the characteristics of remote sensing images, we first use lifting wavelet transform based on adaptive direction evaluation (ADE) to obtain multi-scale orientation contrast feature map (MF). Secondly, the features of color are exploited using the information content analysis to provide a color information map (CIM). Thirdly, feature fusion is used to integrate multi-scale orientation contrast features and color information for generating a saliency map. Finally, an adaptive threshold segmentation algorithm is employed to obtain the ROI. Compared with existing models, our method can not only effectively extract detail of the ROIs, but also effectively remove mistaken detection of the inner parts of the ROIs.

  1. Analysis of the essential oils of Alpiniae Officinarum Hance in different extraction methods (United States)

    Yuan, Y.; Lin, L. J.; Huang, X. B.; Li, J. H.


    It was developed for the analysis of the essential oils of Alpiniae Officinarum Hance extracted by steam distillation (SD), ultrasonic assisted solvent extraction (UAE) and supercritical fluid extraction (SFE) via gas chromatography mass spectrometry (GC-MS) combined with retention index (RI) method. There were multiple volatile components of the oils extracted by the three above-mention methods respectively identified; meanwhile, each one was quantified by area normalization method. The results indicated that the content of 1,8-Cineole, the index constituent, by SD was similar as SFE, and higher than UAE. Although UAE was less time consuming and consumed less energy, the oil quality was poorer due to the use of organic solvents was hard to degrade. In addition, some constituents could be obtained by SFE but could not by SD. In conclusion, essential oil of different extraction methods from the same batch of materials had been proved broadly similarly, however, there were some differences in composition and component ratio. Therefore, development and utilization of different extraction methods must be selected according to the functional requirements of products.

  2. Testing of viable human skin cell dilution cultures as an approach to validating microsampling. (United States)

    Ainger, Stephen A; Yong, X L Hilary; Soyer, H Peter; Sturm, Richard A


    Skin biopsies are a valuable technique in the diagnosis of cutaneous inflammatory and neoplastic conditions. We were interested to test the minimal size or equivalent volume by dilution of proteolytically disassociated skin tissue required to allow the isolation and propagation of cutaneous cells, for freezing, storage and biochemical analysis. It was possible to propagate with 100% efficiency fibroblast and melanocytic cells from a 0.1 to 0.5 mm(3) equivalent neonatal foreskin sample using a combination of DispaseII and CollagenaseIV. The smallest tissue dilution that allowed melanocytic cell culture was 0.01 mm(3), which equated to approximately 16 cells based on the average skin density of melanocytes. However, passaging of cells to create frozen stocks was achieved routinely only from 1 mm(3) skin, equating to 1560 cells. Tissue-specific antigen expression of these cultures was tested by western blot of total protein extracts. There was no pigmentation antigen expression in fibroblast cultures; however, smooth muscle actin protein expression was high in fibroblast but absent from melanocytic cell strains. Melanocytic cells expressed pigmentation antigens and E-cadherin, but these were not detected in fibroblasts. Moreover, maturation of these melanocytic cells resulted in a decrease of Dopachrome Tautomerase antigen expression and induction of Tyrosinase protein consistent with the differentiation potential seen in cell cultures derived routinely from large sections of skin tissue.

  3. Solid Phase Extraction: Applications to the Chromatographic Analysis of Vegetable Oils and Fats

    Energy Technology Data Exchange (ETDEWEB)

    Panagiotopoulout, P. M.; Tsimidou, M.


    Applications of solid-phase extraction for the isolation of certain lipid classes prior to chromatographic analysis are given. More information was found for sterols and related compounds, polar phenols and contaminants such as polycyclic aromatic hydrocarbons. Detailed analytical protocols are presented and discussed in many cases. (Author) 120 refs.

  4. BioFoV - An open platform for forensic video analysis and biometric data extraction

    DEFF Research Database (Denmark)

    Almeida, Miguel; Correia, Paulo Lobato; Larsen, Peter Kastmand


    to tailor-made software, based on state of art knowledge in fields such as soft biometrics, gait recognition, photogrammetry, etc. This paper proposes an open and extensible platform, BioFoV (Biometric Forensic Video tool), for forensic video analysis and biometric data extraction, aiming to host some...


    A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

  6. Chemical analysis and quality control of Ginkgo biloba leaves, extracts, and phytopharmaceuticals

    NARCIS (Netherlands)

    Beek, van T.A.; Montoro, P.


    The chemical analysis and quality control of Ginkgo leaves, extracts, phytopharmaceuticals and some herbal supplements is comprehensively reviewed. The review is an update of a similar, earlier review in this journal [T.A. van Beek, J. Chromatogr. A 967 (2002) 21¿55]. Since 2001 over 3000 papers on


    A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

  8. Spectral analysis and anti-bacterial activity of methanolic fruit extract ...

    African Journals Online (AJOL)

    sunny t

    Gas chromatography-mass spectrometry (GC-MS) analysis of C. colocynthis revealed the existence of the methyl 6-oxoheptanoate, hexanoic acid, .... obtained from an alcoholic extract of colocynth, an ether- ... room temperature with 100 ml of methanol for 6 h according to ..... Plant based natural constituents can be.

  9. Shrimp Allergy: Analysis of Commercially Available Extracts for In Vivo Diagnosis. (United States)

    Asero, R; Scala, E; Villalta, D; Pravettoni, V; Arena, A; Billeri, L; Colombo, G; Cortellini, G; Cucinelli, F; De Cristofaro, M L; Farioli, L; Iemoli, E; Lodi Rizzini, F; Longo, R; Losappio, L; Macchia, D; Maietta, G; Minale, P; Murzilli, F; Nebiolo, F; Pastorello, E A; Ventura, M T; Voltolini, S; Amato, S; Mistrello, G

    Skin prick testing (SPT) with commercial extracts is the first step in the diagnosis of shrimp allergy, although its clinical efficiency is unknown. Objective: To analyze the clinical usefulness of all commercial crustacean extracts available for SPT in Italy. We performed a multicenter study of 157 shrimp-allergic patients who underwent SPT with 5 commercial crustacean extracts and with house dust mite (HDM) extract. Commercial extracts were analyzed using SDS-PAGE and compared with a freshly prepared in-house shrimp extract. IgE to Pen a 1/Pen m 1, Pen m 2, and Pen m 4 was determined, and immunoblot analysis was performed on a large number of sera. The skin reactions caused by commercial crustacean extracts were extremely heterogeneous, resulting in 32 clinical profiles, with marked differences in protein content and missing proteins at molecular weights corresponding to those of major shrimp allergens. Only strong Pen a 1/Pen m 1 reactors reacted to both HDM and all 5 commercial extracts in SPT. Most patients, including those who were tropomyosin-negative, reacted to HDM. Patients reacted to a large and variable array of proteins, and IgE reactivity was common at high molecular weights (>50 kDa). The in vivo diagnosis of shrimp allergy must continue to be based on SPT with fresh material. Shrimp-allergic patients frequently react to a number of ill-defined high-molecular-weight allergens, thus leaving currently available materials for component-resolved diagnosis largely insufficient. Mites and crustaceans probably share several allergens other than tropomyosin.

  10. Solvent effects on quantitative analysis of brominated flame retardants with Soxhlet extraction. (United States)

    Zhong, Yin; Li, Dan; Zhu, Xifen; Huang, Weilin; Peng, Ping'an


    Reliable quantifications of brominated flame retardants (BFRs) not only ensure compliance with laws and regulations on the use of BFRs in commercial products, but also is key for accurate risk assessments of BFRs. Acetone is a common solvent widely used in the analytical procedure of BFRs, but our recent study found that acetone can react with some BFRs. It is highly likely that such reactions can negatively affect the quantifications of BFRs in environmental samples. In this study, the effects of acetone on the extraction yields of three representative BFRs [i.e., decabrominated diphenyl ether (decaBDE), hexabromocyclododecane (HBCD) and tetrabromobisphenol A (TBBPA)] were evaluated in the Soxhlet extraction (SE) system. The results showed that acetone-based SE procedure had no measureable effect for the recovery efficiencies of decaBDE but could substantially lower the extraction yields for both TBBPA and HBCD. After 24 h of extraction, the recovery efficiencies of TBBPA and HBCD by SE were 93 and 78% with acetone, 47 and 70% with 3:1 acetone:n-hexane, and 82 and 94% with 1:1 acetone:n-hexane, respectively. After 72 h of extraction, the extraction efficiencies of TBBPA and HBCD decreased to 68 and 55% with acetone, 0 and 5% with 3:1 acetone/n-hexane mixtures, and 0 and 13% with 1:1 acetone/n-hexane mixtures, respectively. The study suggested that the use of acetone alone or acetone-based mixtures should be restricted in the quantitative analysis of HBCD and TBBPA. We further evaluated nine alternative solvents for the extraction of the three BFRs. The result showed that diethyl ether might be reactive with HBCD and may not be considered as the alternative to acetone used solvents for the extraction of HBCD.


    Directory of Open Access Journals (Sweden)

    Nik Aina Syazana Nik Zainuddin


    Full Text Available Dendrophthoe pentandra known as mistletoe is a semi-parasitic plant with traditional claims for some medicinal properties. This research was done to determine phytochemical constituents of Dendropthoe petandra (DP leaves extract, to evaluate toxicity of extracts by brine shrimp lethality test (BSLT and to confirm cytotoxicity activity of DPME against various normal cell lines. The most potent extract was then evaluated by GC-MS. DP leaves that have been extracted with petroleum ether (DPPEE, methanol (DPME and water (DPWE were screened for phytochemical constituents. BSLT was carried out to determine the lethality concentration that kills 50% of tested population (LC50. The cytotoxicity was assessed by Methylene Blue Assay (MBA that evaluates the inhibition concentration for cell growth by 50% (IC50. The normal cell lines used were MDCK, L929 and Vero. Phytochemical analysis revealed the presence of alkaloid, flavonoid, saponin, tannin and terpenoid in those extracts. Highest total phenolic content was found in DPME (471.63±2.02 mg GAE/g. BSLT have determined the lowest LC50 value is 2.74±1.23 ppm in DPME. No IC50 detected when MDCK, L929 and Vero cell line were treated with all extracts. Therefore, this can be concluded that DP extracts did not show any harmful effects towards MDCK, L929 and Vero cell lines although the DPME, DPPEE and DPWE are toxic towards brine shrimp. Hexadecanoic acid, methyl ester and 9,12,15-Octadecatrienoic acid, methyl ester are among compounds present in DPME. Further studies using mammalian cancer cell lines should be conducted on DP extracts to know if they posses anticancer potential.

  12. Environmental analysis of raw cork extraction in cork oak forests in southern Europe (Catalonia--Spain). (United States)

    Rives, Jesús; Fernandez-Rodriguez, Ivan; Rieradevall, Joan; Gabarrell, Xavier


    Cork oak grows endemically in a narrow region bordering the western Mediterranean, and especially in the Iberian Peninsula. The importance of cork agro-forestry systems lies in the fact that a natural and renewable raw material - cork - can be extracted sustainably without endangering the tree or affecting biodiversity. This paper describes an environmental analysis of the extraction of raw cork in cork oak forests in Catalonia, using data from five representative local forest exploitations. The evaluation was carried out using life cycle assessment (LCA) methodology, and all the forestry management required to obtain a tonne of raw cork was included. The aim of the study was to evaluate the environmental impacts - in terms of global warming, acidification, eutrophication, human toxicity, and so on - caused by cork extraction and determine the carbon dioxide balance of these forestry systems, with a tree lifespan of about 200 years. During the life cycle extraction of cork in Catalonia, 0.2 kg of CO(2) eq. was emitted per kg of raw cork extracted. Moreover, cork cannot be extracted without the tree, which will be fixing carbon dioxide throughout its technological useful life (200 years), despite the fact that the bark is removed periodically: every 13-14 years. If the emission from extraction and the carbon contained in the material is discounted, the carbon dioxide balance indicates that 18 kg of CO(2) are fixed per kg of raw cork extracted. Therefore, cork is a natural, renewable and local material that can replace other non-renewable materials, at local level, to reduce the environmental impacts of products, and particularly to reduce their carbon footprint.

  13. Puffed cereals with added chamomile - quantitative analysis of polyphenols and optimization of their extraction method. (United States)

    Blicharski, Tomasz; Oniszczuk, Anna; Olech, Marta; Oniszczuk, Tomasz; Wójtowicz, Agnieszka; Krawczyk, Wojciech; Nowak, Renata


    [b]Abstract Introduction[/b]. Functional food plays an important role in the prevention, management and treatment of chronic diseases. One of the most interesting techniques of functional food production is extrusion-cooking. Functional foods may include such items as puffed cereals, breads and beverages that are fortified with vitamins, some nutraceuticals and herbs. Due to its pharmacological activity, chamomile flowers are the most popular components added to functional food. Quantitative analysis of polyphenolic antioxidants, as well as comparison of various methods for the extraction of phenolic compounds from corn puffed cereals, puffed cereals with an addition of chamomile (3, 5, 10 and 20%) and from [i]Chamomillae anthodium. [/i] [b]Materials and Methods[/b]. Two modern extraction methods - ultrasound assisted extraction (UAE) at 40 °C and 60 °C, as well as accelerated solvent extraction (ASE) at 100 °C and 120 °C were used for the isolation of polyphenols from functional food. Analysis of flavonoids and phenolic acids was carried out using reversed-phase high-performance liquid chromatography and electrospray ionization mass spectrometry (LC-ESI-MS/MS). [b]Results and Conclusions[/b]. For most of the analyzed compounds, the highest yields were obtained by ultrasound assisted extraction. The highest temperature during the ultrasonification process (60 °C) increased the efficiency of extraction, without degradation of polyphenols. UAE easily arrives at extraction equilibrium and therefore permits shorter periods of time, reducing the energy input. Furthermore, UAE meets the requirements of 'Green Chemistry'.

  14. Improved proteomic analysis following trichloroacetic acid extraction of Bacillus anthracis spore proteins. (United States)

    Deatherage Kaiser, Brooke L; Wunschel, David S; Sydor, Michael A; Warner, Marvin G; Wahl, Karen L; Hutchison, Janine R


    Proteomic analysis of bacterial samples provides valuable information about cellular responses and functions under different environmental pressures. Analysis of cellular proteins is dependent upon efficient extraction from bacterial samples, which can be challenging with increasing complexity and refractory characteristics. While no single method can recover 100% of the bacterial proteins, selected protocols can improve overall protein isolation, peptide recovery, or enrichment for certain classes of proteins. The method presented here is technically simple, does not require specialized equipment such as a mechanical disrupter, and is effective for protein extraction of the particularly challenging sample type of Bacillus anthracis Sterne spores. The ability of Trichloroacetic acid (TCA) extraction to isolate proteins from spores and enrich for spore-specific proteins was compared to the traditional mechanical disruption method of bead beating. TCA extraction improved the total average number of proteins identified within a sample as compared to bead beating (547 vs 495, respectively). Further, TCA extraction enriched for 270 spore proteins, including those typically identified by first isolating the spore coat and exosporium layers. Bead beating enriched for 156 spore proteins more typically identified from whole spore proteome analyses. The total average number of proteins identified was equal using TCA or bead beating for easily lysed samples, such as B. anthracis vegetative cells. As with all assays, supplemental methods such as implementation of an alternative preparation method may simplify sample preparation and provide additional insight to the protein biology of the organism being studied.

  15. Reflux extraction and analysis of polyethylene wax in soil 

    Institute of Scientific and Technical Information of China (English)

    XIONG Xiao-li; CHEN Cheng; LUO Xue-gang


    An efficient reflux extraction of polyethylene wax (PEW) in soil is presented, followed by molecular structure characterization methods to explore its degradation mechanism. To more realistically simulate the actual degradation of PE film powders in soil, low density PE (M=5 000) powders, being used as simulated PEW residue sample, were uniformly mixed with soil and then recovered by reflux extraction with decahydronaphthalen (decalin) at 90°C for 60 min. The average recovery of PEW from fortified soils was 96.5%with the developed reflux extraction procedure. The recovered PEW residue samples were characterized by infrared spectroscopy (IR), element analysis (EA), X-ray fluorescence (XFR), and high-temperature gel permeation chromatography (GPC). The results from spectra analysis show that there were no significant changes in molecular structures and molecular mass distribution of PEW samples after the reflux extraction, which demonstrate the reliability of this method. These results also indicate that the reflux extraction procedure and analytical methods of characterization could serve as a novel measurement technique to evaluate the degradation of low-density PE powders in soil over time.

  16. Rapid extraction of melamine in powdered milk for direct electrospray ionization tandem mass spectrometry analysis. (United States)

    Domingo, Elisângela do Carmo; Tireli, Aline Auxiliadora; Nunes, Cleiton Antonio; Batista, Alexandre Vieira; Guerreiro, Mário César; Pinto, Sandra Maria


    A combination of a simple pretreatment for melamine extraction and direct analysis in electrospray ionization tandem mass spectrometry (ESI-MS/MS) is proposed. Three pretreatments were evaluated. The first was based on suppressing interference using acetonitrile. The second used sulphuric acid and trichloroacetic acid to suppress interference and for melamine extraction, respectively. The third used sulphuric acid to suppress milk interference, trichloroacetic acid for melamine precipitation, and ethyl acetate for melamine extraction. However, only the last pretreatment suppressed milk interference in melamine detection and a good linearity (R(2)=0.99) was obtained. The presence of MS/MS 85 on melamine fragmentation spectrum showed the selectivity of this method. The limit of detection and limit of quantification were 0.269 µg L(-1) and 0.897 µg L(-1), respectively. The recoveries and relative standard deviation (RDS) of method were lower than 114% and 7.86%, respectively. Further, the research was extended to elucidate the nature of the melamine in the extract through infrared spectroscopy and microscopy analyses. The precipitate was characterized as melaminium bis(trichloroacetate) dihydrate, which is generated through hydrogen bound formation in an interaction between melamine and trichloroacetic acid. Therefore, a simple, fast, and easy method for melamine extraction and direct ESI-MS/MS analysis was developed.

  17. Evaluation of four protein extraction methods for proteomic analysis of mango peel. (United States)

    Liao, D J; Lu, X P; Chen, H S; Lu, Y; Mo, Z Y


    The peel of mango (Mangifera indica L.) is a special plant tissue that contains many compounds that interfere with protein extraction. A successful separation with Two-dimensional electrophoresis (2-DE) is the key step for proteomic analysis. To evaluate the efficiencies of mango peel protein extraction for 2-DE, four extraction methods were tested: 1) 2-D clean-up kit, 2) trichloroacetic acid/acetone precipitation, 3) phenol extraction, 4) phenol with methanol/ammonium acetate precipitation. The results showed that the phenol with methanol/ammonium acetate precipitation produced the best quality protein extraction and separation. Proteins were separated in 30-70 and >70 kDa ranges better than with the other methods. Acidic proteins had better resolution with fewer horizontal and vertical streaks. Sixteen proteins were identified by maxtrix-assisted laser desorption/ ionisation time-of-flight tandem mass spectrometry (MALDI-TOF/ TOF-MS/MS). The result demonstrated that each of these four methods can be used to prepare mango peel proteins. The phenol with methanol/ ammonium acetate precipitation was the best choice for proteomic analysis of mango peel.

  18. Extracting a Smooth Trend from a Time Series: A Modification of Singular Spectrum Analysis. (United States)

    Solow, Andrew R.; Patwardhan, Anand


    Singular spectrum analysis is commonly used in climatology to extract a trend from a noisy time series. Implicit in this method is the association of trends with high variance. In many cases, it may be more natural to associate trends with smoothness. This paper describes how singular spectrum analysis can be modified to incorporate this idea. The modified approach is illustrated using the annual central England temperature series.

  19. Small Target Extraction Based on Independent Component Analysis for Hyperspectral Imagery

    Institute of Scientific and Technical Information of China (English)

    LU Wei; YU Xuchu


    A small target detection approach based on independent component analysis for hyperspectral data is put forward. In this algorithm, firstly the fast independent component analysis(FICA) is used to collect target information hided in high-dimensional data and projects them into low-dimensional space.Secondly, the feature images are selected with kurtosis .At last, small targets are extracted with histogram image segmentation which has been labeled by skewness.

  20. Preliminary design and analysis of a process for the extraction of lithium from seawater

    Energy Technology Data Exchange (ETDEWEB)

    Steinberg, M.; Dang, V.D.


    The U.S. demand for lithium by the industrial sector and by a fusion power economy in the future is discussed. For a one million MW(e) CTR (D-T fuel cycle) economy, growing into the beginning of the next century (the years 2000 to 2030), the cumulative demand for lithium is estimated to range from (0.55 to 4.7) x 10/sup 7/ to 1.0 x 10/sup 9/ kg. Present estimates of the available U.S. supply are 6.9 x 10/sup 8/ kg of lithium from mineral resources and 4.0 x 10/sup 9/ kg of lithium from concentrated natural brines. There is, however, a vast supply of lithium in seawater: 2.5 x 10/sup 14/ kg. A preliminary process design for the extraction of lithium from seawater is presented: seawater is first evaporated by solar energy to increase the concentration of lithium and to decrease the concentration of other cations in the bittern which then passes into a Dowex-50 ion exchange bed for cation adsorption. Lithium ions are then eluted with dilute hydrochloric acid forming an aqueous lithium chloride which is subsequently concentrated and electrolyzed. The energy requirement for lithium extraction varies between 0.08 and 2.46 kWh(e)/gm for a range of production rates varying between 10/sup 4/ and 10/sup 8/ kg/y; this is small compared to the energy produced from the use of lithium in a CTR having a value of 3400 kWh(e)/g Li. Production cost of the process is estimated to be in the range of 2.2 to 3.2 cents/g Li. As a basis for the process design, it is recommended that a phase equilibria study of the solid--liquid crystallization processes of seawater be conducted. Uncertainties exist in the operation of large solar ponds for concentrating large quantities of seawater. A search for a highly selective adsorbent or extractant for Li from low concentration aqueous solutions should be made. Other physical separation processes such as using membranes should be investigated. 9 tables. (DLC)

  1. Image Analysis of Soil Micromorphology: Feature Extraction, Segmentation, and Quality Inference

    Directory of Open Access Journals (Sweden)

    Petros Maragos


    Full Text Available We present an automated system that we have developed for estimation of the bioecological quality of soils using various image analysis methodologies. Its goal is to analyze soilsection images, extract features related to their micromorphology, and relate the visual features to various degrees of soil fertility inferred from biochemical characteristics of the soil. The image methodologies used range from low-level image processing tasks, such as nonlinear enhancement, multiscale analysis, geometric feature detection, and size distributions, to object-oriented analysis, such as segmentation, region texture, and shape analysis.

  2. Phase transitions in diluted negative-weight percolation models. (United States)

    Apolo, L; Melchert, O; Hartmann, A K


    We investigate the geometric properties of loops on two-dimensional lattice graphs, where edge weights are drawn from a distribution that allows for positive and negative weights. We are interested in the appearance of spanning loops of total negative weight. The resulting percolation problem is fundamentally different from conventional percolation, as we have seen in a previous study of this model for the undiluted case. Here, we investigate how the percolation transition is affected by additional dilution. We consider two types of dilution: either a certain fraction of edges exhibits zero weight, or a fraction of edges is even absent. We study these systems numerically using exact combinatorial optimization techniques based on suitable transformations of the graphs and applying matching algorithms. We perform a finite-size scaling analysis to obtain the phase diagram and determine the critical properties of the phase boundary. We find that the first type of dilution does not change the universality class compared to the undiluted case whereas the second type of dilution leads to a change in the universality class.

  3. Phytochemical analysis of the flower extracts of Rhododendron arboreum Sm. ssp. nilagiricum (Zenker) Tagg

    Institute of Scientific and Technical Information of China (English)

    Kiruba S; Mahesh M; Nisha SR; Miller Paul Z; Jeeva S


    Objective: To evaluate the preliminary phytochemical screening of the flower extracts of Rhododendron arboreum (R. arboreum) Sm. ssp. nilagiricum (Zenker) Tagg. Methods: The preliminary phytochemical screening was performed by the standard methods as described by Harborne. Results: The phytochemical analysis carried out on the flowers of R. arboreum Sm. ssp. nilagiricum (Zenker) Tagg showed the presence of phenols, saponins, steroids, tannin, xanthoprotein and coumarin. Conclusions:The present study suggested that the flower extracts of R. arboreum Sm. ssp. nilagiricum (Zenker) Tagg possess significant phytochemical constituents and it can be used as antimicrobial agents against clinically isolated pathogens.

  4. A kinetic analysis of strand breaks on large DNA induced by cigarette smoke extract (United States)

    Kurita, Hirofumi; Takata, Tatsuya; Yasuda, Hachiro; Takashima, Kazunori; Mizuno, Akira


    We report a kinetic analysis of strand breakages on large DNA molecules induced by cigarette smoke extract (CSE), an extract of soluble cigarette smoke components. Previously, this DNA damage was analyzed by agarose gel electrophoresis, whereas we used fluorescence to kinetically analyze damage to individual DNA molecules. CSE caused a marked change in length of DNA molecules. The rate of CSE-induced double-strand breakage on large random-coiled DNA molecules was determined using a simple theoretical model, allowing the facile estimation of the rate of double-strand breaks on large DNA molecules.

  5. Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography (United States)

    Belisle, A.A.; Swineford, D.M.


    A simple, specific procedure was developed for the analysis of organophosphorus and carbamate pesticides in sediment. The wet soil was mixed with anhydrous sodium sulfate to bind water and the residues were column extracted in acetone:methylene chloride (1:l,v/v). Coextracted water was removed by additional sodium sulfate packed below the sample mixture. The eluate was concentrated and analyzed directly by capillary gas chromatography using phosphorus and nitrogen specific detectors. Recoveries averaged 93 % for sediments extracted shortly after spiking, but decreased significantly as the samples aged.

  6. Analysis of Automated Modern Web Crawling and Testing Tools and Their Possible Employment for Information Extraction

    Directory of Open Access Journals (Sweden)

    Tomas Grigalis


    Full Text Available World Wide Web has become an enormously big repository of data. Extracting, integrating and reusing this kind of data has a wide range of applications, including meta-searching, comparison shopping, business intelligence tools and security analysis of information in websites. However, reaching information in modern WEB 2.0 web pages, where HTML tree is often dynamically modified by various JavaScript codes, new data are added by asynchronous requests to the web server and elements are positioned with the help of cascading style sheets, is a difficult task. The article reviews automated web testing tools for information extraction tasks.Article in Lithuanian


    CERN Document Server

    Abernethy, Samuel


    Within CERN's accelerator complex, the extraction from the Proton Synchrotron to the Super Proton Synchrotron has been done using the so-called ``Continuous Transfer" (CT) method since the 1970's. A new technique, known as Multi-Turn Extraction (MTE), has now been implemented and is in full operation. This report examines a holistic performance analysis of the novel technique in multiple aspects of the accelerator complex, as well as a direct comparison with its predecessor, CT, from the implementation of MTE in 2010 until the end of 2015.

  8. A microfluidic cigarette smoke collecting platform for simultaneous sample extraction and multiplex analysis. (United States)

    Hu, Shan-Wen; Xu, Bi-Yi; Qiao, Shu; Zhao, Ge; Xu, Jing-Juan; Chen, Hong-Yuan; Xie, Fu-Wei


    In this work, we report a novel microfluidic gas collecting platform aiming at simultaneous sample extraction and multiplex mass spectrometry (MS) analysis. An alveolar-mimicking elastic polydimethylsiloxane (PDMS) structures was designed to move dynamically driven by external pressure. The movement was well tuned both by its amplitude and rhythm following the natural process of human respiration. By integrating the alveolar units into arrays and assembling them to gas channels, a cyclic contraction/expansion system for gas inhale and exhale was successfully constructed. Upon equipping this system with a droplet array on the alveolar array surface, we were able to get information of inhaled smoke in a new strategy. Here, with cigarette smoke as an example, analysis of accumulation for target molecules during passive smoking is taken. Relationships between the breathing times, distances away from smokers and inhaled content of nicotine are clarified. Further, by applying different types of extraction solvent droplets on different locations of the droplet array, simultaneous extraction of nicotine, formaldehyde and caproic acid in sidestream smoke (SS) are realized. Since the extract droplets are spatially separated, they can be directly analyzed by MS which is fast and can rid us of all complex sample separation and purification steps. Combining all these merits, this small, cheap and portable platform might find wide application in inhaled air pollutant analysis both in and outdoors. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Selective production of hemicellulose-derived carbohydrates from wheat straw using dilute HCl or FeCl3 solutions under mild conditions. X-ray and thermo-gravimetric analysis of the solid residues. (United States)

    Marcotullio, G; Krisanti, E; Giuntoli, J; de Jong, W


    The present work explores the combined production of hemicellulose-derived carbohydrates and an upgraded solid residue from wheat straw using a dilute-acid pretreatment at mild temperature. Dilute aqueous HCl solutions were studied at temperatures of 100 and 120°C, and they were compared to dilute FeCl(3) under the same conditions. Comparable yields of soluble sugars and acetic acid were obtained, affording an almost complete removal of pentoses when using 200 mM aqueous solutions at 120°C. The solid residues of pretreatment were characterized showing a preserved crystallinity of the cellulose, and a almost complete removal of ash forming matter other than Si. Results showed upgraded characteristic of the residues for thermal conversion applications compared to the untreated wheat straw.

  10. Extracting aluminum from dross tailings (United States)

    Amer, A. M.


    Aluminum dross tailings, an industrial waste, from the Egyptian Aluminium Company (Egyptalum) was used to produce two types of alums: aluminum-sulfate alum [itAl2(SO4)3.12H2O] and ammonium-aluminum alum [ (NH 4)2SO4AL2(SO4)3.24H2O]. This was carried out in two processes. The first process is leaching the impurities using diluted H2SO4 with different solid/liquid ratios at different temperatures to dissolve the impurities present in the starting material in the form of solute sulfates. The second process is the extraction of aluminum (as aluminum sulfate) from the purifi ed aluminum dross tailings thus produced. The effects of temperature, time of reaction, and acid concentration on leaching and extraction processes were studied. The product alums were analyzed using x-ray diffraction and thermal analysis techniques.

  11. Development of a microwave assisted extraction method for the analysis of 2,4,6-trichloroanisole in cork stoppers by SIDA-SBSE-GC-MS

    Energy Technology Data Exchange (ETDEWEB)

    Vestner, Jochen [Forschungsanstalt Geisenheim, Fachgebiet Mikrobiologie und Biochemie, Von-Lade-Strasse 1, D-65366 Geisenheim (Germany); Hochschule RheinMain, Fachbereich Geisenheim, Von-Lade-Strasse 1, D-65366 Geisenheim (Germany); Fritsch, Stefanie [Forschungsanstalt Geisenheim, Fachgebiet Mikrobiologie und Biochemie, Von-Lade-Strasse 1, D-65366 Geisenheim (Germany); Rauhut, Doris, E-mail: [Forschungsanstalt Geisenheim, Fachgebiet Mikrobiologie und Biochemie, Von-Lade-Strasse 1, D-65366 Geisenheim (Germany)


    The aim of this research work was focused on the replacement of the time-consuming soaking of cork stoppers which is mainly used as screening method for cork lots in connection with sensory analysis and/or analytical methods to detect releasable 2,4,6-trichloroanisole (TCA) of natural cork stoppers. Releasable TCA from whole cork stoppers was analysed with the application of a microwave assisted extraction method (MAE) in combination with stir bar sorptive extraction (SBSE). The soaking of corks (SOAK) was used as a reference method to optimise MAE parameters. Cork lots of different quality and TCA contamination levels were used to adapt MAE. Pre-tests indicated that an MAE at 40 deg. C for 120 min with 90 min of cooling time are suitable conditions to avoid an over-extraction of TCA of low and medium tainted cork stoppers in comparison to SOAK. These MAE parameters allow the measuring of almost the same amounts of releasable TCA as with the application of the soaking procedure in the relevant range (<25 ng L{sup -1} releasable TCA from one cork) to evaluate the TCA level of cork stoppers. Stable isotope dilution assay (SIDA) was applied to optimise quantification of the released TCA with deuterium-labelled TCA (TCA-d{sub 5}) using a time-saving GC-MS technique in single ion monitoring (SIM) mode. The developed MAE method allows the measuring of releasable TCA from the whole cork stopper under improved conditions and in connection with a low use of solvent and a higher sample throughput.

  12. A simple method of genomic DNA extraction from human samples for PCR-RFLP analysis. (United States)

    Ghatak, Souvik; Muthukumaran, Rajendra Bose; Nachimuthu, Senthil Kumar


    Isolation of DNA from blood and buccal swabs in adequate quantities is an integral part of forensic research and analysis. The present study was performed to determine the quality and the quantity of DNA extracted from four commonly available samples and to estimate the time duration of the ensuing PCR amplification. Here, we demonstrate that hair and urine samples can also become an alternate source for reliably obtaining a small quantity of PCR-ready DNA. We developed a rapid, cost-effective, and noninvasive method of sample collection and simple DNA extraction from buccal swabs, urine, and hair using the phenol-chloroform method. Buccal samples were subjected to DNA extraction, immediately or after refrigeration (4-6°C) for 3 days. The purity and the concentration of the extracted DNA were determined spectrophotometerically, and the adequacy of DNA extracts for the PCR-based assay was assessed by amplifying a 1030-bp region of the mitochondrial D-loop. Although DNA from all the samples was suitable for PCR, the blood and hair samples provided a good quality DNA for restriction analysis of the PCR product compared with the buccal swab and urine samples. In the present study, hair samples proved to be a good source of genomic DNA for PCR-based methods. Hence, DNA of hair samples can also be used for the genomic disorder analysis in addition to the forensic analysis as a result of the ease of sample collection in a noninvasive manner, lower sample volume requirements, and good storage capability.

  13. The antibacterial activity of diluted Tualang honey

    Directory of Open Access Journals (Sweden)

    N. A. Roslan


    Full Text Available Tualang honey (TH is a Malaysian jungle honey obtained from the wild. The honey is produced by the rock bee (Apis dorsata, which builds hives on branches of tall Tualang (Koompassia excelsa (Becc. Taub trees located mainly in the north-western region of Peninsular Malaysia. Limited information is available on the antibacterial mechanism of local honey. The present study was conducted to determine the antibacterial activity of diluted ?Tualang? honey against Escherichia coli (E. coli. Three different Tualang honey concentrations, namely, 20, 30 and 40% were used to examine the effect of diluting Tualang honey on its antibacterial effect towards E. coli. The 40% diluted honey was the most effective in inhibiting the growth of E. coli, followed by honey diluted at 20 and 30%. The high antibacterial activity of honey towards E. Coli was thought to arise from the production of hydrogen peroxide, but requires further study to validate the action.

  14. Extraction, Identification and Quantitative HPLC Analysis of Flavonoids From Fruit Extracts of Arbutus unedo L from Tiaret Area (Western Algeria

    Directory of Open Access Journals (Sweden)

    Khadidja Bouzid


    Full Text Available The aim of the current study was to evaluate the total phenolic, flavonoid content and to investigate the antioxidant capacities of the fruit extracts of Arbutus unedo L. that grows in Tiaret area (Western Algeria. First we have extracted the fruit by some non-polar solvent (chloroform, ethyl acetate, 1-butanol. Total phenolic content and total flavonoid content were evaluated according to the Folin-Ciocalteu procedure, and a colorimetric method, respectively. Extracts content was determined by using a high-performance liquid chromatography (HPLC-UV method. The total phenolic contents of A.unedo L. varied between 12.75±0.06 to 34.17±1.36 mg gallic acid equivalent/g of dry weight of extract. The total flavonoid varied from 2.18±0.10 to 6.54±1.14 mg catechin equivalent/g. The antioxidant potential of all extracts was evaluated using 1,1-diphenyl-2-picrylhydrazyl (DPPH free radical scavenging activity, the IC50 of acetate ethyl was the best by 0,009 mg/ml may due to the phenolic compound, in the second was the chloroform extract by IC50=0,015mg/ml, in the third was butanol extract by IC50= 0,022 mg/ml and in the last was water extract by IC50= 0,048mg/ml. the antioxidant activity of all extracts was better than ascorbic acid. The extract obtained under optimum conditions was analyzed by HPLC and five flavonoid compounds were identified; they are catechin, apiginin, silybin, fisetine and naringin.

  15. Preliminary phytochemical analysis, antibacterial, antifungal and anticandidal activities of successive extracts of Crossandra infundibuliformis

    Institute of Scientific and Technical Information of China (English)

    MadhumithaG; SaralAM


    Objective:To investigate the phytochemical, antibacterial, antifungal and anticandidal activity of successive extracts of Crossandra infundibuliformis (Acanthaceae) leaves. Methods:Preliminary screening on the presence of alkaloids, saponins, phytosterols, phenolic compounds, flavanoids, tannins, carbohydrates, terpenoids, oils and fats were carried out by phytochemical analysis. The antibacterial, antifungal and anticandidal activities were done by agar well diffusion technique. Results:The successive extracts have an array of chemical constituents and the MIC values of antibacterial activity ranges from 0.007 8 to 0.015 0μg/mL. In case of antifungal and anticandidal activities the MIC values were between 0.125 and 0.250μg/mL. Conclusions:These findings demonstrate that the leaf extracts of C. infundibuliformis presents excellent antimicrobial activities and thus have great potential as a source for natural health care products.

  16. Automated DNA extraction of single dog hairs without roots for mitochondrial DNA analysis. (United States)

    Bekaert, Bram; Larmuseau, Maarten H D; Vanhove, Maarten P M; Opdekamp, Anouschka; Decorte, Ronny


    Dogs are intensely integrated in human social life and their shed hairs can play a major role in forensic investigations. The overall aim of this study was to validate a semi-automated extraction method for mitochondrial DNA analysis of telogenic dog hairs. Extracted DNA was amplified with a 95% success rate from 43 samples using two new experimental designs in which the mitochondrial control region was amplified as a single large (± 1260 bp) amplicon or as two individual amplicons (HV1 and HV2; ± 650 and 350 bp) with tailed-primers. The results prove that the extraction of dog hair mitochondrial DNA can easily be automated to provide sufficient DNA yield for the amplification of a forensically useful long mitochondrial DNA fragment or alternatively two short fragments with minimal loss of sequence in case of degraded samples.

  17. Feature Extraction of Gesture Recognition Based on Image Analysis for Different Environmental Conditions

    Directory of Open Access Journals (Sweden)

    Rahul A. Dedakiya


    Full Text Available Gesture recognition system received great attention in the recent few years because of its manifoldness applications and the ability to interact with machine efficiently through human computer interaction. Gesture is one of human body languages which are popularly used in our daily life. It is a communication system that consists of hand movements and facial expressions via communication by actions and sights. This research mainly focuses on the research of gesture extraction and finger segmentation in the gesture recognition. In this paper, we have used image analysis technologies to create an application by encoding in MATLAB program. We will use this application to segment and extract the finger from one specific gesture. This paper is aimed to give gesture recognition in different natural conditions like dark and glare condition, different distances condition and similar object condition then collect the results to calculate the successful extraction rate.

  18. Combining the quick, easy, cheap, effective, rugged and safe approach and clean-up by immunoaffinity column for the analysis of 15 mycotoxins by isotope dilution liquid chromatography tandem mass spectrometry. (United States)

    Desmarchelier, Aurélien; Tessiot, Sabine; Bessaire, Thomas; Racault, Lucie; Fiorese, Elisa; Urbani, Alessandro; Chan, Wai-Chinn; Cheng, Pearly; Mottier, Pascal


    Optimization and validation of a multi-mycotoxin method by LC-MS/MS is presented. The method covers the EU-regulated mycotoxins (aflatoxins, fumonisins, ochratoxin A, deoxynivalenol, zearalenone, T-2 and HT-2), as well as nivalenol and 3- and 15-acetyldeoxynivalenol for analysis of cereals, cocoa, oil, spices, infant formula, coffee and nuts. The proposed procedure combines two clean-up strategies: First, a generic preparation suitable for all mycotoxins based on the QuEChERS (for quick, easy, cheap, effective, rugged and safe) protocol. Second, a specific clean-up devoted to aflatoxins and ochratoxin A using immunoaffinity column (IAC) clean-up. Positive identification of mycotoxins in matrix was conducted according to the confirmation criteria defined in EU Commission Decision 2002/657/EC while quantification was performed by isotopic dilution using (13)C-labeled mycotoxins as internal standards. Limits of quantification were at or below the maximum levels set in the EC/1886/2006 document for all mycotoxin/matrix combinations under regulation. In particular, the inclusion of an IAC step allowed achieving LOQs as low as 0.05 and 0.25μg/kg in cereals for aflatoxins and ochratoxin A, respectively. Other performance parameters like linearity [(r)(2)>0.99], recovery [71-118%], precision [(RSDr and RSDiR)<33%], and trueness [78-117%] were all compliant with the analytical requirements stipulated in the CEN/TR/16059 document. Method ruggedness was proved by a verification process conducted by another laboratory. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Phylogenetic spectrum and analysis of antibacterial activities of leaf extracts from plants of the genus Rhododendron. (United States)

    Rezk, Ahmed; Nolzen, Jennifer; Schepker, Hartwig; Albach, Dirk C; Brix, Klaudia; Ullrich, Matthias S


    Plants are traditionally used for medicinal treatment of numerous human disorders including infectious diseases caused by microorganisms. Due to the increasing resistance of many pathogens to commonly used antimicrobial agents, there is an urgent need for novel antimicrobial compounds. Plants of the genus Rhododendron belong to the woody representatives of the family Ericaceae, which are typically used in a range of ethno-medical applications. There are more than one thousand Rhododendron species worldwide. The Rhododendron-Park Bremen grows plants representing approximately 600 of the known Rhododendron species, and thus enables research involving almost two thirds of all known Rhododendron species. Twenty-six bacterial species representing different taxonomic clades have been used to study the antimicrobial potential of Rhododendron leaf extracts. Agar diffusion assay were conducted using 80% methanol crude extracts derived from 120 Rhododendron species. Data were analyzed using principal component analysis and the plant-borne antibacterial activities grouped according the first and second principal components. The leaf extracts of 17 Rhododendron species exhibited significant growth-inhibiting activities against Gram-positive bacteria. In contrast, only very few of the leaf extracts affected the growth of Gram-negative bacteria. All leaf extracts with antimicrobial bioactivity were extracted from representatives of the subgenus Rhododendron, with 15 from the sub-section Rhododendron and two belonging to the section Pogonanthum. The use of bacterial multidrug efflux pump mutants revealed remarkable differences in the susceptibility towards Rhododendron leaf extract treatment. For the first time, our comprehensive study demonstrated that compounds with antimicrobial activities accumulate in the leaves of certain Rhododendron species, which mainly belong to a particular subgenus. The results suggested that common genetic traits are responsible for the production of

  20. Plant extracts for the topical management of psoriasis: a systematic review and meta-analysis. (United States)

    Deng, S; May, B H; Zhang, A L; Lu, C; Xue, C C L


    Patients with psoriasis frequently use preparations of plant extracts. Physicians need to be aware of the current evidence concerning these products. This review evaluates the efficacy and safety of preparations of plant extracts used topically for psoriasis. Searches were conducted in PubMed, Embase, the Cochrane library, two Chinese databases and article reference lists. Randomized controlled trials investigating extracts of single plants were included. Preparations of multiple plants and combinations of plant extracts plus conventional therapies were excluded. Two authors conducted searches, extracted data and assessed risk of bias. Outcomes used in meta-analyses were: clinical efficacy, Psoriasis Area and Severity Index score, and quality of life and symptom scores. The 12 included studies investigated extracts of: Mahonia aquifolium (n = 5), Aloe vera (n = 3), indigo naturalis (n = 2), kukui nut oil (n = 1) and Camptotheca acuminata nut (n = 1). Methodological quality was variable. Six studies provided data suitable for meta-analysis of clinical efficacy, and five were vs. placebo (relative risk 3·37, 95% confidence interval 1·36-8·33). Experimental studies indicate components of indigo naturalis, Mahonia and Camptotheca have anti-inflammatory, antiproliferative and other actions of relevance to psoriasis. The clinical trial evidence provides limited support for preparations containing extracts of M. aquifolium, indigo naturalis and Aloe vera for the topical management of plaque psoriasis based on multiple studies. No serious adverse events were reported. Because of the small size of most studies and methodological weaknesses, strong conclusions cannot be made. The magnitudes of any effects cannot be measured with accuracy, so it is difficult to assess the clinical relevance of these preparations.

  1. Comparing DNA extraction methods for analysis of botanical materials found in anti-diabetic supplements. (United States)

    Llongueras, Jose P; Nair, Saraswathy; Salas-Leiva, Dayana; Schwarzbach, Andrea E


    A comparative performance evaluation of DNA extraction methods from anti-diabetic botanical supplements using various commercial kits was conducted, to determine which produces the best quality DNA suitable for PCR amplification, sequencing and species identification. All plant materials involved were of suboptimal quality showing various levels of degradation and therefore representing real conditions for testing herbal supplements. Eight different DNA extraction methods were used to isolate genomic DNA from 13 medicinal plant products. Two methods for evaluation, DNA concentration measurements that included absorbance ratios as well as PCR amplifiability, were used to determine quantity and quality of extracted DNA. We found that neither DNA concentrations nor commonly used UV absorbance ratio measurements at A(260)/A(280) between 1.7 and 1.9 are suitable for globally predicting PCR success in these plant samples, and that PCR amplifiablity itself was the best indicator of extracted product quality. However, our results suggest that A(260)/A(280) ratios below about 1.3 and above 2.3 indicated a DNA quality too poor to amplify. Therefore, A(260)/A(280) measurements are not useful to identify samples that likely will amplify but can be used to exclude samples that likely will not amplify reducing the cost for unnecessarily subjecting samples to PCR. The two Nucleospin(®) plant II kit extraction methods produced the most pure and amplifiable genomic DNA extracts. Our results suggest that there are clear, discernable differences between extraction methods for low quality plant samples in terms of producing contamination-free, high-quality genomic DNA to be used for further analysis.

  2. [Dan'e-fukang soft extract for dysmenorrhea: a meta-analysis]. (United States)

    Yu, Kun; Zhang, Zhen-dong; Xiao, Zheng; Wei, Wei; Wang, Zheng-long


    To assess the efficacy and safety of Dan'e-fukang soft extract for dysmenorrhea by meta-analysis. Cochrane Controlled Trials Register, PubMed, EMBASE, CBM, VIP, Wanfang Data, and CNKI databases were searched. Results of randomized controlled trials were also harvested from pharmaceutical companies by manual search. Meta-analysis was carried out according to the method provided by the Cochrane Collaboration with RevMan5.0 software. Twelve Chinese papers were selected, and 1213 patients were included. Significant difference in recovery rate was found between Dan'e-fukang soft extract group and other drugs group (RR=1.33, 95%CI: 1.02-1.75, P0.05). No statistical difference was noticed in total effective rate between two groups (RR=1.04, 95%CI: 1.00-1.08, P>0.05). A statistical difference in improvement of dysmenorrhea symptoms was found before and after treatment in both Dan'e-fukang soft extract group and other drugs group (MD=5.79, 95%CI: 5.01-6.56, P0.05) and after treatment (MD=-0.94, 95%CI: -2.11-0.23, P>0.05). Oral administration of Dan'e-fukang soft extract caused only mild gastrointestinal discomfort, but other drugs had more adverse effects including serious gastrointestinal reaction, severe liver dysfunction, vaginal bleeding, and female masculinity. The existing evidence shows that Dan'e-fukang soft extract has the same efficacy as other drugs in treatment of dysmenorrheal. Because of the quality of the included studies was limited, the evidence of the efficacy and safety of Dan'e-fukang soft extract was not strong, and high-quality randomized trials with large samples are needed.

  3. Comparison of two commercial DNA extraction kits for the analysis of nasopharyngeal bacterial communities

    Directory of Open Access Journals (Sweden)

    Keith A. Crandall


    Full Text Available Characterization of microbial communities via next-generation sequencing (NGS requires an extraction ofmicrobial DNA. Methodological differences in DNA extraction protocols may bias results and complicate inter-study comparisons. Here we compare the effect of two commonly used commercial kits (Norgen and Qiagenfor the extraction of total DNA on estimatingnasopharyngeal microbiome diversity. The nasopharynxis a reservoir for pathogens associated with respiratory illnesses and a key player in understandingairway microbial dynamics. Total DNA from nasal washes corresponding to 30 asthmatic children was extracted using theQiagenQIAamp DNA and NorgenRNA/DNA Purification kits and analyzed via IlluminaMiSeq16S rRNA V4 ampliconsequencing. The Norgen samples included more sequence reads and OTUs per sample than the Qiagen samples, but OTU counts per sample varied proportionallybetween groups (r = 0.732.Microbial profiles varied slightly between sample pairs, but alpha- and beta-diversity indices (PCoAand clustering showed highsimilarity between Norgen and Qiagenmicrobiomes. Moreover, no significant differences in community structure (PERMANOVA and adonis tests and taxa proportions (Kruskal-Wallis test were observed betweenkits. Finally, aProcrustes analysis also showed low dissimilarity (M2 = 0.173; P< 0.001 between the PCoAs of the two DNA extraction kits. Contrary to what has been observed in previous studies comparing DNA extraction methods, our 16S NGS analysis of nasopharyngeal washes did not reveal significant differences in community composition or structure between kits. Our findingssuggest congruence between column-based chromatography kits and supportthe comparison of microbiomeprofilesacross nasopharyngeal metataxonomic studies.

  4. Chemical Analysis of Extracts from Newfoundland Berries and Potential Neuroprotective Effects

    Directory of Open Access Journals (Sweden)

    Mohammad Z. Hossain


    Full Text Available Various species of berries have been reported to contain several polyphenolic compounds, such as anthocyanins and flavonols, which are known to possess high antioxidant activity and may be beneficial for human health. To our knowledge, a thorough chemical analysis of polyphenolics in species of these plants native to Newfoundland, Canada has not been conducted. The primary objective of this study was to determine the polyphenolic compounds present in commercial extracts from Newfoundland berries, which included blueberries (V. angustifolium, lingonberries (V. vitis-idaea and black currant (Ribes lacustre. Anthocyanin and flavonol glycosides in powdered extracts from Ribes lacustre and the Vaccinium species were identified using the high performance liquid chromatographic (HPLC separation method with mass spectrometric (MS detection. The identified compounds were extracted from dried berries by various solvents via ultrasonication followed by centrifugation. A reverse-phase analytical column was employed to identify the retention time of each chemical component before submission for LC–MS analysis. A total of 21 phenolic compounds were tentatively identified in the three species. Further, we tested the effects of the lingonberry extract for its ability to protect neurons and glia from trauma utilizing an in vitro model of cell injury. Surprisingly, these extracts provided complete protection from cell death in this model. These findings indicate the presence of a wide variety of anthocyanins and flavonols in berries that grow natively in Newfoundland. These powdered extracts maintain these compounds intact despite being processed from berry fruit, indicating their potential use as dietary supplements. In addition, these recent findings and previous data from our lab demonstrate the ability of compounds in berries to protect the nervous system from traumatic insults.

  5. Comparison of Different Protein Extraction Methods for Gel-Based Proteomic Analysis of Ganoderma spp. (United States)

    Al-Obaidi, Jameel R; Saidi, Noor Baity; Usuldin, Siti Rokhiyah Ahmad; Hussin, Siti Nahdatul Isnaini Said; Yusoff, Noornabeela Md; Idris, Abu Seman


    Ganoderma species are a group of fungi that have the ability to degrade lignin polymers and cause severe diseases such as stem and root rot and can infect economically important plants and perennial crops such as oil palm, especially in tropical countries such as Malaysia. Unfortunately, very little is known about the complex interplay between oil palm and Ganoderma in the pathogenesis of the diseases. Proteomic technologies are simple yet powerful tools in comparing protein profile and have been widely used to study plant-fungus interaction. A critical step to perform a good proteome research is to establish a method that gives the best quality and a wide coverage of total proteins. Despite the availability of various protein extraction protocols from pathogenic fungi in the literature, no single extraction method was found suitable for all types of pathogenic fungi. To develop an optimized protein extraction protocol for 2-DE gel analysis of Ganoderma spp., three previously reported protein extraction protocols were compared: trichloroacetic acid, sucrose and phenol/ammonium acetate in methanol. The third method was found to give the most reproducible gels and highest protein concentration. Using the later method, a total of 10 protein spots (5 from each species) were successfully identified. Hence, the results from this study propose phenol/ammonium acetate in methanol as the most effective protein extraction method for 2-DE proteomic studies of Ganoderma spp.

  6. A comprehensive method for extraction and quantitative analysis of sterols and secosteroids from human plasma. (United States)

    McDonald, Jeffrey G; Smith, Daniel D; Stiles, Ashlee R; Russell, David W


    We describe the development of a method for the extraction and analysis of 62 sterols, oxysterols, and secosteroids from human plasma using a combination of HPLC-MS and GC-MS. Deuterated standards are added to 200 μl of human plasma. Bulk lipids are extracted with methanol:dichloromethane, the sample is hydrolyzed using a novel procedure, and sterols and secosteroids are isolated using solid-phase extraction (SPE). Compounds are resolved on C₁₈ core-shell HPLC columns and by GC. Sterols and oxysterols are measured using triple quadrupole mass spectrometers, and lathosterol is measured using GC-MS. Detection for each compound measured by HPLC-MS was ∪ 1 ng/ml of plasma. Extraction efficiency was between 85 and 110%; day-to-day variability showed a relative standard error of <10%. Numerous oxysterols were detected, including the side chain oxysterols 22-, 24-, 25-, and 27-hydroxycholesterol, as well as ring-structure oxysterols 7α- and 4β-hydroxycholesterol. Intermediates from the cholesterol biosynthetic pathway were also detected, including zymosterol, desmosterol, and lanosterol. This method also allowed the quantification of six secosteroids, including the 25-hydroxylated species of vitamins D₂ and D₃. Application of this method to plasma samples revealed that at least 50 samples could be extracted in a routine day.

  7. Phytochemical analysis with the antioxidant and aldose reductase inhibitory capacities of Tephrosia humilis aerial parts' extracts. (United States)

    Plioukas, Michael; Gabrieli, Chrysi; Lazari, Diamanto; Kokkalou, Eugene


    The aerial parts of Tephrosia humilis were tested about their antioxidant potential, their ability to inhibit the aldose/aldehyde reductase enzymes and their phenolic content. The plant material was exhaustively extracted with petroleum ether, dichloromethane and methanol, consecutively. The concentrated methanol extract was re-extracted, successively, with diethyl ether, ethyl acetate and n-butanol. All extracts showed significant antioxidant capacity, but the most effective was the ethyl acetate extract. As about the aldose reductase inhibition, all fractions, except the aqueous, were strong inhibitors of the enzyme, with the n-butanolic and ethyl acetate fractions to inhibit the enzyme above 75%. These findings provide support to the ethnopharmacological usage of the plant as antioxidant and validate its potential to act against the long-term diabetic complications. The phytochemical analysis showed the presence of 1,4-dihydroxy-3,4-(epoxyethano)-5-cyclohexene(1), cleroindicin E(2), lupeol(3), methyl p-coumarate(4), methyl 4-hydroxybenzoate(5), prunin(6), 5,7,2',5'-tetrahydroxyflavanone 7-rutinoside(7), protocatechuic acid(8), luteolin 7-glucoside(9), apigenin(10), naringin(11), rhoifolin(12) and luteolin 7-glucuronate(13).

  8. Revealing the metabonomic variation of rosemary extracts using 1H NMR spectroscopy and multivariate data analysis. (United States)

    Xiao, Chaoni; Dai, Hui; Liu, Hongbing; Wang, Yulan; Tang, Huiru


    The molecular compositions of rosemary ( Rosmarinus officinalis L.) extracts and their dependence on extraction solvents, seasons, and drying processes were systematically characterized using NMR spectroscopy and multivariate data analysis. The results showed that the rosemary metabonome was dominated by 33 metabolites including sugars, amino acids, organic acids, polyphenolic acids, and diterpenes, among which quinate, cis-4-glucosyloxycinnamic acid, and 3,4,5-trimethoxyphenylmethanol were found in rosemary for the first time. Compared with water extracts, the 50% aqueous methanol extracts contained higher levels of sucrose, succinate, fumarate, malonate, shikimate, and phenolic acids, but lower levels of fructose, glucose, citrate, and quinate. Chloroform/methanol was an excellent solvent for selective extraction of diterpenes. From February to August, the levels of rosmarinate and quinate increased, whereas the sucrose level decreased. The sun-dried samples contained higher concentrations of rosmarinate, sucrose, and some amino acids but lower concentrations of glucose, fructose, malate, succinate, lactate, and quinate than freeze-dried ones. These findings will fill the gap in the understanding of rosemary composition and its variations.

  9. Analysis on the Physicochemical Properties of Ginkgo biloba Leaves after Enzymolysis Based Ultrasound Extraction and Soxhlet Extraction. (United States)

    Zhang, Chang-Wei; Wang, Cheng-Zhang; Tao, Ran


    In this study, high performance liquid chromatography (HPLC), ultraviolet (UV), thermagravimetric analyzer (TGA), pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS), and scanning electron microscope (SEM) were used as measurement techniques, contents of chemical composition, pyrolytic products, thermal stability, morphological characterization of Ginkgo biloba leaves (GBL) acted as the index, and physicochemical properties of GBL after enzymolysis based ultrasound extraction (EBUE) and Soxhlet extraction were studied. The detection results of chemical composition revealed that contents of general flavone, soluble protein, soluble total sugar and protein in the GBL declined significantly after EBUE, and contents of polyprenols and crude fat obviously reduced as well after Soxhlet extraction. Py-GC-MS results indicated that total GC contents of micromolecules with carbon less than 12 from 54.0% before EBUE decline to 8.34% after EBUE. Total GC contents of long-chain fatty acids with carbon less than 20 from 43.0% before EBUE reduced to 27.0% after Soxhlet extraction. Thermal stability results showed that GBL after Soxhlet extraction was easier to decompose than GBL before EBUE. SEM results illustrated that surface structure of GBL was damaged severely after EBUE, compared with GBL before EBUE, while organic solvent extraction had little influence on the morphological characterization of GBL after Soxhlet extraction compared with GBL after EBUE.

  10. Analysis on the Physicochemical Properties of Ginkgo biloba Leaves after Enzymolysis Based Ultrasound Extraction and Soxhlet Extraction

    Directory of Open Access Journals (Sweden)

    Chang-Wei Zhang


    Full Text Available In this study, high performance liquid chromatography (HPLC, ultraviolet (UV, thermagravimetric analyzer (TGA, pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS, and scanning electron microscope (SEM were used as measurement techniques, contents of chemical composition, pyrolytic products, thermal stability, morphological characterization of Ginkgo biloba leaves (GBL acted as the index, and physicochemical properties of GBL after enzymolysis based ultrasound extraction (EBUE and Soxhlet extraction were studied. The detection results of chemical composition revealed that contents of general flavone, soluble protein, soluble total sugar and protein in the GBL declined significantly after EBUE, and contents of polyprenols and crude fat obviously reduced as well after Soxhlet extraction. Py-GC-MS results indicated that total GC contents of micromolecules with carbon less than 12 from 54.0% before EBUE decline to 8.34% after EBUE. Total GC contents of long-chain fatty acids with carbon less than 20 from 43.0% before EBUE reduced to 27.0% after Soxhlet extraction. Thermal stability results showed that GBL after Soxhlet extraction was easier to decompose than GBL before EBUE. SEM results illustrated that surface structure of GBL was damaged severely after EBUE, compared with GBL before EBUE, while organic solvent extraction had little influence on the morphological characterization of GBL after Soxhlet extraction compared with GBL after EBUE.

  11. Regularized generalized eigen-decomposition with applications to sparse supervised feature extraction and sparse discriminant analysis

    DEFF Research Database (Denmark)

    Han, Xixuan; Clemmensen, Line Katrine Harder


    techniques, for instance, 2D-Linear Discriminant Analysis (2D-LDA). Furthermore, an iterative algorithm based on the alternating direction method of multipliers is developed. The algorithm approximately solves RGED with monotonically decreasing convergence and at an acceptable speed for results of modest......We propose a general technique for obtaining sparse solutions to generalized eigenvalue problems, and call it Regularized Generalized Eigen-Decomposition (RGED). For decades, Fisher's discriminant criterion has been applied in supervised feature extraction and discriminant analysis...... accuracy. Numerical experiments based on four data sets of different types of images show that RGED has competitive classification performance with existing multidimensional and sparse techniques of discriminant analysis....

  12. Comparison of DNA Extraction Methods for Microbial Community Analysis in Indonesian Tempe Employing Amplified Ribosomal Intergenic Spacer Analysis

    Directory of Open Access Journals (Sweden)



    Full Text Available Tempe fermentation involved complex microbial communities which are only revealed partially through culture dependent methods. Culture-independent methods would be potential to unravel this complex microbial fermentation. Appropriate DNA extraction is an essential tool to obtain reliable data from culture independent method. In this study, we employed two commercial DNA extraction methods to find the best one for microbial community characterization employing amplified ribosomal intergenic spacer analysis (ARISA. Our result showed that PowerFood Microbial DNA Isolation Kit-MOBIO (PFMDIK is an excellent method for microbial DNA extraction from tempe. It gave high quantity and quality of DNA suitable for PCR amplification of 16S-23S rRNA intergenic spacer to yield a diverse and reproducible ARISA profile.

  13. Efficiency of EGFR mutation analysis for small microdissected cytological specimens using multitech DNA extraction solution. (United States)

    Oh, Seo Young; Lee, Hoon Taek


    The microdissection method has greatly facilitated the isolation of pure cell populations for accurate analysis of mutations. However, the absence of coverslips in these preparations leads to poor resolution of cellular morphological features. In the current study, the authors developed the MultiTech DNA extraction solution to improve the visualization of cell morphology for microdissection and tested it for the preservation of morphological properties of cells, quality of DNA, and ability to detect mutations. A total of 121 cytological samples, including fine-needle aspirates, sputum, pleural fluid, and bronchial washings, were selected from hospital archives. DNA extracted from microdissected cells was evaluated by epidermal growth factor receptor (EGFR) mutation analysis using pyrosequencing, Sanger sequencing, and peptide nucleic acid (PNA)-mediated real-time polymerase chain reaction clamping. Morphological features of cells as well as DNA quality and quantity were analyzed in several cytological samples to assess the performance of the MultiTech DNA extraction solution. The results were compared with previous EGFR mutation tests. The MultiTech DNA extraction solution improved the morphology of archived stained cells before microdissection and provided a higher DNA yield than the commercial QIAamp DNA Mini Kit in samples containing a minimal number of cells (25-50 cells). The authors were able to detect identical EGFR mutations by using different analysis platforms and consistently identified these mutations in samples comprising as few as 25 microdissected cells. The MultiTech DNA extraction solution is a reliable medium that improves the resolution of cell morphology during microdissection. It was particularly useful in EGFR mutations of samples containing a small number of cells. © 2015 American Cancer Society.

  14. Evaluation of extraction procedures for 2-DE analysis of aphid proteins. (United States)

    Yiou, Pan; Shaoli, An; Kebin, Li; Tao, Wang; Kui, Fang; Hua, Zhang; Yu, Sun; Xun, Yang; Jinghui, Xi


    Protein sample preparation is a crucial step in a 2-DE proteomics approach. In order to establish a routine protocol for the application of proteomics analysis to aphids, this study focuses on the specific protein extraction problems in insect tissues and evaluates four methods to bypass them. The approaches of phenol extraction methanol/ammonium acetate precipitation (PA), TCA/acetone precipitation, PEG precipitation, and no precipitation were evaluated for proteins isolation and purification from apterous adult aphids, Sitobion avenae. For 2-DE, the PA protocol was optimal, resulting in good IEF and clear spots. PA method yielded the greatest amount of protein and displayed most protein spots in 2-DE gels, as compared with the TCA/acetone precipitation, PEG precipitation and no precipitation protocols. Analysis of protein yield, image quality and spot numbers demonstrate that the TCA/acetone precipitation protocol is a reproducible and reliable method for extracting proteins from aphids. The PEG precipitation approach is a newly developed protein extraction protocol for aphids, from which more unique protein spots can be detected, especially for detection of acid proteins. These protocols are expected to be applicable to other insects or could be of interest to laboratories involved in insect proteomics, despite the amounts and types of interfering compounds vary considerably in different insects.

  15. Antimicrobial Activity and Chromatographic Analysis of Extracts from Tropaeolum pentaphyllum Lam. Tubers

    Directory of Open Access Journals (Sweden)

    Ritiel Corrêa da Cruz


    Full Text Available Background: Tropaeolum pentaphyllum Lam. tubers (Tropaeolaceae are known and used as a condiment and for the treatment of skin infections in Southern Brazil. However, its activity and composition has not yet been investigated. Thus, different extracts and the essential oil from the tubers were tested against a range of microorganisms. The most active extracts were submitted to chromatographic analysis. Methods: Hydroalcoholic extract (70%, fractions of it, and the essential oil from the tubers were tested against several bacteria, yeasts and molds, furnishing the corresponding inhibitory, bactericidal and fungicidal minimal concentration values. The most active extracts were submitted to GC-MS investigation. Results: The strongest effects against different strains of microorganisms, such as Gram-positive and negative bacteria, Candida spp. and dermatophytes were observed for the essential oil and the chloroform fraction, with minimal inhibitory concentrations (MICs well below 200 µg/mL. GC-MS analysis revealed that the major essential oil constituent is benzyl isothiocyanate (BITC, while the chloroform fraction is constituted of BITC, amides, sulfur, fatty acids and its esters, all compounds that may be related to the demonstrated activity. Conclusions: Overall, the results support the popular use of the plant for the treatment of skin infections, and revealed the main active compounds.

  16. Text Region Extraction: A Morphological Based Image Analysis Using Genetic Algorithm

    Directory of Open Access Journals (Sweden)

    Dhirendra Pal Singh


    Full Text Available Image analysis belongs to the area of computer vision and pattern recognition. These areas are also a part of digital image processing, where researchers have a great attention in the area of content retrieval information from various types of images having complex background, low contrast background or multi-spectral background etc. These contents may be found in any form like texture data, shape, and objects. Text Region Extraction as a content from an mage is a class of problems in Digital Image Processing Applications that aims to provides necessary information which are widely used in many fields medical imaging, pattern recognition, Robotics, Artificial intelligent Transport systems etc. To extract the text data information has becomes a challenging task. Since, Text extraction are very useful for identifying and analysis the whole information about image, Therefore, In this paper, we propose a unified framework by combining morphological operations and Genetic Algorithms for extracting and analyzing the text data region which may be embedded in an image by means of variety of texts: font, size, skew angle, distortion by slant and tilt, shape of the object which texts are on, etc. We have established our proposed methods on gray level image sets and make qualitative and quantitative comparisons with other existing methods and concluded that proposed method is better than others.

  17. On statistical analysis of factors affecting anthocyanin extraction from Ixora siamensis (United States)

    Mat Nor, N. A.; Arof, A. K.


    This study focused on designing an experimental model in order to evaluate the influence of operative extraction parameters employed for anthocyanin extraction from Ixora siamensis on CIE color measurements (a*, b* and color saturation). Extractions were conducted at temperatures of 30, 55 and 80°C, soaking time of 60, 120 and 180 min using acidified methanol solvent with different trifluoroacetic acid (TFA) contents of 0.5, 1.75 and 3% (v/v). The statistical evaluation was performed by running analysis of variance (ANOVA) and regression calculation to investigate the significance of the generated model. Results show that the generated regression models adequately explain the data variation and significantly represented the actual relationship between the independent variables and the responses. Analysis of variance (ANOVA) showed high coefficient determination values (R2) of 0.9687 for a*, 0.9621 for b* and 0.9758 for color saturation, thus ensuring a satisfactory fit of the developed models with the experimental data. Interaction between TFA content and extraction temperature exhibited to the highest significant influence on CIE color parameter.

  18. Comparative Proteomic Analysis of Cotton Fiber Development and Protein Extraction Method Comparison in Late Stage Fibers

    Directory of Open Access Journals (Sweden)

    Hana Mujahid


    Full Text Available The distinct stages of cotton fiber development and maturation serve as a single-celled model for studying the molecular mechanisms of plant cell elongation, cell wall development and cellulose biosynthesis. However, this model system of plant cell development is compromised for proteomic studies due to a lack of an efficient protein extraction method during the later stages of fiber development, because of a recalcitrant cell wall and the presence of abundant phenolic compounds. Here, we compared the quality and quantities of proteins extracted from 25 dpa (days post anthesis fiber with multiple protein extraction methods and present a comprehensive quantitative proteomic study of fiber development from 10 dpa to 25 dpa. Comparative analysis using a label-free quantification method revealed 287 differentially-expressed proteins in the 10 dpa to 25 dpa fiber developmental period. Proteins involved in cell wall metabolism and regulation, cytoskeleton development and carbohydrate metabolism among other functional categories in four fiber developmental stages were identified. Our studies provide protocols for protein extraction from maturing fiber tissues for mass spectrometry analysis and expand knowledge of the proteomic profile of cotton fiber development.

  19. Comprehensive analysis of drugs of abuse in urine using disposable pipette extraction. (United States)

    Ellison, Sparkle T; Brewer, William E; Morgan, Stephen L


    The extraction of basic, acidic, and neutral drugs of abuse from a low volume of urine (0.2 mL) using disposable pipette extraction (DPX) is described. DPX is a solid-phase extraction device that uses loosely contained sorbent inside a pipette tip fitted with a screen. This device provides faster extraction times because conditioning steps are not required. In this study, the DPX used a modified divinyl benzene sorbent containing both cation-exchange and reversed-phase mechanisms that facilitates the retention of basic and acidic/neutral drugs, respectively. With this device, a comprehensive method of analysis was developed for a diverse group of drugs and drug classes in urine including amphetamines, opiates, cocaine and its metabolites, tetrahydrocannabinol metabolite, tricyclic antidepressants, meperidine, methadone, and phencyclidine. Recoveries of the majority of drugs analyzed were 90% or greater with relative standard deviations of less than 10%. Additional validation involved the analysis of urine specimens previously analyzed by a local forensic toxicology laboratory.

  20. [Extraction and analysis of nuclear DNA from free margin of nail material]. (United States)

    Nie, Sheng-Jie; Yang, Yan-Mei; Tang, Wen-Ru; Xu, Bing-Ying; Jing, Qiang; Xiao, Chun-Jie


    To investigate the feasibility of DNA analysis from free margin of the nail, genomic DNA was extracted from the free margin of nail clipping of 10 volunteers using the proteinase K/SDS -based organic method, the Chelex-100 method, or a combined method. Target DNA was simultaneously amplified using a fluorescent multiplex AmpFlSTR Identifier kit. The PCR products were analyzed on the ABI PRISM 3130 Genetic Analyzer. The results showed that, compared with profiles achieved by genotyping of blood samples from each volunteer as reference, 100% concordance was achieved using the combined method. The STR genotype profiles obtained through the organic method were acceptable, despite preferential amplification at some loci. In contrast, no readable profiles could be determined when DNA was extracted by the Chelex-100 method, and there were a large number of alleles missing. Our data suggest that free margin of nail can be used for nuclear DNA analysis, but the type of DNA isolation method used is critical. The traditional organic extraction method works reasonably well for free margin nail DNA isolation, and combination of organic extraction and the Chelex-100 method works best.

  1. Quantitative analysis of perfumes in talcum powder by using headspace sorptive extraction. (United States)

    Ng, Khim Hui; Heng, Audrey; Osborne, Murray


    Quantitative analysis of perfume dosage in talcum powder has been a challenge due to interference of the matrix and has so far not been widely reported. In this study, headspace sorptive extraction (HSSE) was validated as a solventless sample preparation method for the extraction and enrichment of perfume raw materials from talcum powder. Sample enrichment is performed on a thick film of poly(dimethylsiloxane) (PDMS) coated onto a magnetic stir bar incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace vial by using a holder. The stir bar is then thermally desorbed online with capillary gas chromatography-mass spectrometry. The HSSE method is based on the same principles as headspace solid-phase microextraction (HS-SPME). Nevertheless, a relatively larger amount of extracting phase is coated on the stir bar as compared to SPME. Sample amount and extraction time were optimized in this study. The method has shown good repeatability (with relative standard deviation no higher than 12.5%) and excellent linearity with correlation coefficients above 0.99 for all analytes. The method was also successfully applied in the quantitative analysis of talcum powder spiked with perfume at different dosages. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. An improved high-throughput lipid extraction method for the analysis of human brain lipids. (United States)

    Abbott, Sarah K; Jenner, Andrew M; Mitchell, Todd W; Brown, Simon H J; Halliday, Glenda M; Garner, Brett


    We have developed a protocol suitable for high-throughput lipidomic analysis of human brain samples. The traditional Folch extraction (using chloroform and glass-glass homogenization) was compared to a high-throughput method combining methyl-tert-butyl ether (MTBE) extraction with mechanical homogenization utilizing ceramic beads. This high-throughput method significantly reduced sample handling time and increased efficiency compared to glass-glass homogenizing. Furthermore, replacing chloroform with MTBE is safer (less carcinogenic/toxic), with lipids dissolving in the upper phase, allowing for easier pipetting and the potential for automation (i.e., robotics). Both methods were applied to the analysis of human occipital cortex. Lipid species (including ceramides, sphingomyelins, choline glycerophospholipids, ethanolamine glycerophospholipids and phosphatidylserines) were analyzed via electrospray ionization mass spectrometry and sterol species were analyzed using gas chromatography mass spectrometry. No differences in lipid species composition were evident when the lipid extraction protocols were compared, indicating that MTBE extraction with mechanical bead homogenization provides an improved method for the lipidomic profiling of human brain tissue.

  3. Proximity graph analysis for linear networks extraction from high-resolution satellite imagery (United States)

    Skourikhine, Alexei N.


    Reliable and accurate methods for detection and extraction of linear network, such as road networks, in satellite imagery are essential to many applications. We present an approach to the road network extraction from high-resolution satellite imagery that is based on proximity graph analysis. We are jumping off from the classification provided by existing spectral and textural classification tools, which produce a set of candidate road patches. Then, constrained Delaunay triangulation and Chordal Axis transform are used to extract centerline characterization of the delineated candidate road patches. We refine produced center lines to reduce noise influence on patch boundaries, resulting in a smaller set of robust center lines authentically representing their road patches. Refined center lines are triangulated using constrained Delaunay triangulation (CDT) algorithm to generate a sub-optimal mesh of interconnections among them. The generated triangle edges connecting different center lines are used for spatial analysis of the center lines relations. A subset of the Delaunay tessellation grid contains the Euclidian Minimum Spanning Tree (EMST) that provides an approximation of road network. The approach can be generalized to the multi-criteria MST and multi-criteria shortest path algorithms to integrate other factors important for road network extraction, in addition to proximity relations considered by standard EMST.

  4. [Allergy to cypress pollen: preparation of a reference and standardization extract in vivo]. (United States)

    Leduc, V; Charpin, D; Aparicio, C; Veber, C; Guérin, L


    Development of Cypress allergy frequency led to the standardization of commercial cypress extract used for diagnosis and immunotherapy. Previous in vitro studies on two cypress pollen species (Cupressus sempervirens and Cupressus arizonica) allowed us to produce an allergenic solution composed by a mixture of both extracts for in vivo standardization. Dilutions of this allergenic solution were tested by prick-test on 44 patients with clinical allergy to cypress pollen to define the dilution that corresponds to a 6 mm wheal conformed to the definition of 100 IR. The mixture of the two major species found in France is justified by the in vitro study results. Extracts revealed complementary allergenic composition: Cup sempervirens showed a wider diversity of allergens whereas Cup arizonica showed a higher content of the major 43 kDa allergen. Thus, according to in vivo analysis, we are able to produce a standardized extract of Cypress pollen expressed in IR.

  5. Analysis of Flavonoid in Medicinal Plant Extract Using Infrared Spectroscopy and Chemometrics

    Directory of Open Access Journals (Sweden)

    Lestyo Wulandari


    Full Text Available Infrared (IR spectroscopy combined with chemometrics has been developed for simple analysis of flavonoid in the medicinal plant extract. Flavonoid was extracted from medicinal plant leaves by ultrasonication and maceration. IR spectra of selected medicinal plant extract were correlated with flavonoid content using chemometrics. The chemometric method used for calibration analysis was Partial Last Square (PLS and the methods used for classification analysis were Linear Discriminant Analysis (LDA, Soft Independent Modelling of Class Analogies (SIMCA, and Support Vector Machines (SVM. In this study, the calibration of NIR model that showed best calibration with R2 and RMSEC value was 0.9916499 and 2.1521897, respectively, while the accuracy of all classification models (LDA, SIMCA, and SVM was 100%. R2 and RMSEC of calibration of FTIR model were 0.8653689 and 8.8958149, respectively, while the accuracy of LDA, SIMCA, and SVM was 86.0%, 91.2%, and 77.3%, respectively. PLS and LDA of NIR models were further used to predict unknown flavonoid content in commercial samples. Using these models, the significance of flavonoid content that has been measured by NIR and UV-Vis spectrophotometry was evaluated with paired samples t-test. The flavonoid content that has been measured with both methods gave no significant difference.

  6. Solute dilution at the Borden and Cape Cod groundwater tracer tests (United States)

    Thierrin, Joseph; Kitanidis, Peter K.


    This study presents an analysis of the rate of dilution of a conservative nonreactive tracer in two well-known field experiments: The Borden (Ontario, Canada) experiment and the Cape Cod (Massachusetts) experiment. In evaluating the dilution of injected sodium bromide, in addition to computing the second spatial moments, we have used the dilution index and the reactor ratio. The dilution index is a measure of the formation volume occupied by the solute plume, and the reactor ratio is a shape factor, which measures how stretched and deformed the plume is. Unlike the second moments, which may go up or down during an experiment, the dilution index should increase monotonically. The results for both plumes were quite similar. After an initial period the dilution index increased linearly with time, which is macroscopically equivalent to transport in two-dimensional uniform flow. The reactor ratio was relatively constant during the period of the experiments. Their values, about 0.72 for the Borden test and 0.63 for the Cape Cod test, indicate that the Cape Cod plume was more stretched and deformed than the Borden plume. The maximum concentration, which is an alternative to the dilution index for quantifying dilution, was found to be more erratic and more susceptible to sampling error.

  7. Computation of dilution discharge and mean concentration of effluents in Beypore Estuary, west coast of India

    Digital Repository Service at National Institute of Oceanography (India)

    DineshKumar, P.K.; Josanto, V.; Sankaranarayanan, V.N.

    Tide dominated Beypore estuary along the west coast of India was studied to estimate the mean flow available for diluting the conservative effluents based on the distribution of ambient salinity as a guide through one dimensional analysis...

  8. Determination of Uranium and Plutonium Concentration in 1AF by Isotopic Dilution Mass Spectrometry Methods

    Institute of Scientific and Technical Information of China (English)


    <正>It is important data to measure uranium and plutonium concentration for the reprocessing plant control analysis. The determination of uranium and plutonium concentration in 1AF by isotopic dilution mass

  9. Rapid and automated analysis of aflatoxin M1 in milk and dairy products by online solid phase extraction coupled to ultra-high-pressure-liquid-chromatography tandem mass spectrometry. (United States)

    Campone, Luca; Piccinelli, Anna Lisa; Celano, Rita; Pagano, Imma; Russo, Mariateresa; Rastrelli, Luca


    This study reports a fast and automated analytical procedure for the analysis of aflatoxin M1 (AFM1) in milk and dairy products. The method is based on the simultaneous protein precipitation and AFM1 extraction, by salt-induced liquid-liquid extraction (SI-LLE), followed by an online solid-phase extraction (online SPE) coupled to ultra-high-pressure-liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis to the automatic pre-concentration, clean up and sensitive and selective determination of AFM1. The main parameters affecting the extraction efficiency and accuracy of the analytical method were studied in detail. In the optimal conditions, acetonitrile and NaCl were used as extraction/denaturant solvent and salting-out agent in SI-LLE, respectively. After centrifugation, the organic phase (acetonitrile) was diluted with water (1:9 v/v) and purified (1mL) by online C18 cartridge coupled with an UHPLC column. Finally, selected reaction monitoring (SRM) acquisition mode was applied to the detection of AFM1. Validation studies were carried out on different dairy products (whole and skimmed cow milk, yogurt, goat milk, and powder infant formula), providing method quantification limits about 25 times lower than AFM1 maximum levels permitted by EU regulation 1881/2006 in milk and dairy products for direct human consumption. Recoveries (86-102%) and repeatability (RSDdairy products studied. The proposed method improves the performance of AFM1 analysis in milk samples as AFM1 determination is performed with a degree of accuracy higher than the conventional methods. Other advantages are the reduction of sample preparation procedure, time and cost of the analysis, enabling high sample throughput that meet the current concerns of food safety and the public health protection.

  10. A Unified Factors Analysis Framework for Discriminative Feature Extraction and Object Recognition

    Directory of Open Access Journals (Sweden)

    Ningbo Hao


    Full Text Available Various methods for feature extraction and dimensionality reduction have been proposed in recent decades, including supervised and unsupervised methods and linear and nonlinear methods. Despite the different motivations of these methods, we present in this paper a general formulation known as factor analysis to unify them within a common framework. During factor analysis, an object can be seen as being comprised of content and style factors, and the objective of feature extraction and dimensionality reduction is to obtain the content factor without style factor. There are two vital steps in factor analysis framework; one is the design of factor separating objective function, including the design of partition and weight matrix, and the other is the design of space mapping function. In this paper, classical Linear Discriminant Analysis (LDA and Locality Preserving Projection (LPP algorithms are improved based on factor analysis framework, and LDA based on factor analysis (FA-LDA and LPP based on factor analysis (FA-LPP are proposed. Experimental results show the superiority of our proposed approach in classification performance compared to classical LDA and LPP algorithms.

  11. Ionic Liquid of Infinite Dilution Activity Coefficient Nonlinear Modeling Measurement Process Analysis%离子液体的无限稀释活度系数测量过程分析

    Institute of Scientific and Technical Information of China (English)

    孟玲菊; 玄兆坤; 焦连升


    离子液体受到结构上不对称性、静电作用等多种作用影响,系数特征容易发生形变,传统的测量方法在干扰状态下,很难准确测量.提出一种新的无限稀释活度系数测量模型(MCS-SVM).通过实验测量与无限稀释活度系数相关的溶质参数,并将它们分成为训练集和测试集;然后将训练集输入到一种最小二乘支持向量机分类模型,并测量活度系数,完成最优的无限稀释活度系数测量,消除测量误差.仿真结果表明,相对于传统测量方法可以准确描述无限稀释活度系数与溶质参数的非线性关系,提高了无限稀释活度系数的测量精度.%In order to improve prediction accuracy of the infinite dilution activity coefficient in ion liquid,a prediction model for infinite dilution activity coefficient based on cuckoo search algorithm and least squares support vector machine(MCS-SVM) is proposed.Firstly,the solute parameters of coefficients at infinite dilution are measured and divides into training set and test set; and then the training are input to the least squares support vector machine to train,and the cuckoo search algorithm is used to optimize the parameters of least squares support vector machine.Finally the optimal prediction model of the infinite dilution activity coefficient is established,and the simulation experiments were carried out to test the performance of model.The simulation results show that,compared with the multiple linear regression model and BP neural network,MCS-LSSVM can accurately describe the nonlinear relationship between the infinite dilution activity coefficient and solute parameters,and has improved the prediction accuracy of infinite dilution activity coefficient,provides a new research approach for infinite dilution activity coefficient which has the nonlinear characteristics.

  12. Isolation of Gossypol and Analysis of Phytochemicals in Seed Extract of Bt and Non-Bt Varieties of Cotton

    Directory of Open Access Journals (Sweden)



    Full Text Available The purpose of this study was to isolate the gossypol (Phenolic compound and screening of phytochemical constituents from seed extract. During this study gossypol was extracted from cotton seeds and cotton seed cake using different organic solvents like acetone, ethanol, methanol, pet ether, chloroform and hot water and screened for phytochemical constituents. Analysis revealed the presence of phenols, glycosides, flavonoids, and steroids. Specific tests were conducted for each group of the phytochemicals. Among the extracts tested polar solvents like acetone, ethanol, methanol extracts showed more phytochemicals than others followed by pet ether, hot water, chloroform. The phytochemicals like saponins, flavonoids, tri-terpenoids, and tannins were not found in seed extract, specifically showed phenols with more quantity in polar solvent extract like acetone, ethanol and methanol cardiac glycosides and steroids are observed in both polar and non-polar solvent of seed extracts. Similar kind of compounds are present in Bt and non-Bt but the appearance of test coloration of seed extracts predicted as is slightly darker for Bt variety. This could be due to more amount of the component may be present in Bt cotton seed extract than non-Bt cotton seed extract. The compound Gossypol was detected in extracts by applying Chromatographic technique as well as chemical tests with antimony chloride (SbCl3, and stannic chloride (SnCl3 and leadacetate (Pb(CH3COO2 . Spectrophotometric techniques were also employed for quantitative analysis by measuring absorbance of samples at wavelength of 290nm.

  13. Extraction and isotopic analysis of medium molecular weight hydrocarbons from Murchison using supercritical carbon dioxide (United States)

    Gilmour, Iain; Pillinger, Colin


    The large variety of organic compounds present in carbonaceous chondrites poses particular problems in their analysis not the least of which is terrestrial contamination. Conventional analytical approaches employ simple chromatographic techniques to fractionate the extractable compounds into broad classes of similar chemical structure. However, the use of organic solvents and their subsequent removal by evaporation results in the depletion or loss of semi-volatile compounds as well as requiring considerable preparative work to assure solvent purity. Supercritical fluids have been shown to provide a powerful alternative to conventional liquid organic solvents used for analytical extractions. A sample of Murchison from the Field Museum was analyzed. Two interior fragments were used; the first (2.85 g) was crushed in an agate pestel and mortar to a grain size of ca. 50-100 micron, the second (1.80 g) was broken into chips 3-8