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Sample records for standard thin-layer chromatography

  1. Marker based standardization of polyherbal formulation (SJT-DI-02 by high performance thin layer chromatography method

    Directory of Open Access Journals (Sweden)

    Bhakti J Ladva

    2014-01-01

    purity of the bands due to marker compounds in the sample extracts were confirmed by overlaying the absorption spectra recorded at start, middle and end position of the band in the sample tracks. After conforming all these things fingerprints were developed for all three formulations which will be act as authentification and quality control tool. Results: % w/w of asarones is 3.61, % w/w of marmelosin is 4.60, % w/w of gallic acid is 10.80 and % w/w of lupeol is 4.13.The method was validated in terms of linearity, precision, repeatability, limit of detection, limit of quantification and accuracy. In well-developed mobile phase system linearity was found to be in the range of 0.983-0.995, % recovery was found to be in the range of 97.48-99.63, % RSD for intraday and interday was found to be 0.13- 0.70 and 0.32 -1.41 and LOD and LOQ was found to be in the range of 0.15- 0.61 and 0.45 -1.83 microgram per ml. Conclusion: Thus High performance thin layer chromatography (HPTLC methods were developed and validated in terms of linearity, precision, repeatability, limit of detection, limit of quantification and accuracy. The methods were rapid, sensitive, reproducible and economical. It does not suffer any positive or negative interference due to common other component present in the formulation and would also serve as a tool for authentication of herbal products containing marmelosin, gallic acid, lupeol and asarones. Thus this work provides standardized and therapeutically active polyherbal formulations for the different ailments.

  2. Pre-staining thin layer chromatography method for amino acid ...

    African Journals Online (AJOL)

    The modified thin layer chromatography can be used for the analysis of amino acids. When compared to the classical thin layer chromatography, the improved method was more rapid and inexpensive and the results obtained were clean and reproducible. However, it is suitable for the high throughput screening of amino ...

  3. Pre-staining thin layer chromatography method for amino acid ...

    African Journals Online (AJOL)

    Jane

    2010-12-13

    Dec 13, 2010 ... The modified thin layer chromatography can be used for the analysis of amino acids. When compared to the classical thin layer ... amino acid-producing microbes as well as amino acid fermentation processes. ... sodium hydroxide solution to a final concentration of 0.01M. The fermentation broth was directly.

  4. Isolation, characterization and thin-layer chromatography method development of clerosterol palmityl ester: a chemical marker for standardization of leaves of Clerodendrum phlomidis.

    Science.gov (United States)

    Mohan Maruga Raja, Muthu Kumaradoss; Mishra, Shri Hari

    2012-01-01

    Clerosterol palmityl ester (CPE) is a unique clerosterol derivative isolated and characterized from the leaves of Clerodendrum phlomidis. Considering the uniqueness of this compound, the present study was planned to use CPE as a specific chemical marker and develop a new validated thin-layer chromatography (TLC) method for standardisation of C. phlomidis. Separation and quantification of CPE were achieved by TLC using a mobile phase of petroleum ether (60 to 80 degrees centigrade) and ethyl acetate (95:5, volume ratio) (Rf 0.64) on precoated silica gel 60F(254) aluminium plates. Densitometric determination was carried out after derivatization with anisaldehyde sulphuric acid reagent in absorption mode at 527 nm. The calibration curve was linear in the concentration range of 100 to 500 ng/spot. The method was validated for precision, repeatability and accuracy. The proposed method was found to be simple, specific, precise, accurate, rapid and cost-effective. This TLC procedure may be used effectively for quantitative determination of CPE, identification of the plant and standardization of this plant or its derived products.

  5. Development of High Performance Thin Layer Chromatography for ...

    African Journals Online (AJOL)

    and validation, a high performance thin layer chromatography (HPTLC) system with WinCATS software was used. Freshly prepared ... recommended in routine analysis of pharmaceutical products containing lamivudine and tenofovir disoproxil fumarate. Introduction ... A strong system of quality control and quality assurance ...

  6. Thin-Layer Chromatography: The "Eyes" of the Organic Chemist

    Science.gov (United States)

    Dickson, Hamilton; Kittredge, Kevin W.; Sarquis, Arlyne

    2004-01-01

    Thin-layer chromatography (TLC) methods are successfully used in many areas of research and development such as clinical medicine, forensic chemistry, biochemistry, and pharmaceutical analysis as TLC is relatively inexpensive and has found widespread application as an easy to use, reliable, and quick analytic tool. The usefulness of TLC in organic…

  7. A Thin Layer Chromatography Laboratory Experiment of Medical Importance

    Science.gov (United States)

    Sharma, Loretta; Desai, Ankur; Sharma, Ajit

    2006-01-01

    A thin layer chromatography experiment of medical importance is described. The experiment involves extraction of lipids from simulated amniotic fluid samples followed by separation, detection, and scanning of the lecithin and sphingomyelin bands on TLC plates. The lecithin-to-sphingomyelin ratio is calculated. The clinical significance of this…

  8. 21 CFR 862.2270 - Thin-layer chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Thin-layer chromatography system for clinical use... Instruments § 862.2270 Thin-layer chromatography system for clinical use. (a) Identification. A thin-layer chromatography (TLC) system for clinical use is a device intended to separate one or more drugs or compounds from...

  9. Thin-layer chromatography and colorimetric analysis of multi-component explosive mixtures

    Science.gov (United States)

    Pagoria, Philip F.; Mitchell, Alexander R.; Whipple, Richard E.; Carman, M. Leslie

    2014-08-26

    A thin-layer chromatography method for detection and identification of common military and peroxide explosives in samples includes the steps of provide a reverse-phase thin-layer chromatography plate; prepare the plate by marking spots on which to deposit the samples by touching the plate with a marker; spot one micro liter of a first standard onto one of the spots, spot one micro liter of a second standard onto another of the spots, and spot samples onto other of spots producing a spotted plate; add eluent to a developing chamber; add the spotted plate to the developing chamber; remove the spotted plate from the developing chamber producing a developed plate; place the developed plate in an ultraviolet light box; add a visualization agent to a dip tank; dip the developed plate in the dip tank and remove the developed plate quickly; and detect explosives by viewing said developed plate.

  10. Thin layer chromatography-ion mobility spectrometry (TLC-IMS).

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    Ilbeigi, Vahideh; Tabrizchi, Mahmoud

    2015-01-06

    Ion mobility spectrometry (IMS) is a fast and sensitive analytical method which operates at the atmospheric pressure. To enhance the capability of IMS for the analysis of mixtures, it is often used with preseparation techniques, such as GC or HPLC. Here, we report for the first time the coupling of the thin-layer chromatography and IMS. A variety of coupling schemes were tried that included direct electrospray from the TLC strip tip, indirect electrospray from a needle connected to the TLC strip, introducing the moving solvent into the injection port, and, the simplest way, offline introduction of scratched or cut pieces of strips into the IMS injection port. In this study a special solvent tank was designed and the TLC strip was mounted horizontally where the solvent would flow down. A very small funnel right below the TLC tip collected the solvent and transferred it to a needle via a capillary tubing. Using the TLC-ESI-IMS technique, acceptable separations were achieved for two component mixtures of morphine-papaverine and acridine-papaverine. A special injection port was designed to host the pieces cut off the TLC. The method was successfully used to identify each spot on the TLC by IMS in a few seconds.

  11. Normal and Reversed-Phase Thin Layer Chromatography of Green Leaf Extracts

    Science.gov (United States)

    Sjursnes, Birte Johanne; Kvittingen, Lise; Schmid, Rudolf

    2015-01-01

    Introductory experiments of chromatography are often conducted by separating colored samples, such as inks, dyes, and plant extracts, using filter paper, chalk, or thin layer chromatography (TLC) plates with various solvent systems. Many simple experiments have been reported. The relationship between normal chromatography and reversed-phase…

  12. Frontally eluted components procedure with thin layer chromatography as a mode of sample preparation for high performance liquid chromatography quantitation of acetaminophen in biological matrix.

    Science.gov (United States)

    Klimek-Turek, A; Sikora, M; Rybicki, M; Dzido, T H

    2016-03-04

    A new concept of using thin-layer chromatography to sample preparation for the quantitative determination of solute/s followed by instrumental techniques is presented Thin-layer chromatography (TLC) is used to completely separate acetaminophen and its internal standard from other components (matrix) and to form a single spot/zone containing them at the solvent front position (after the final stage of the thin-layer chromatogram development). The location of the analytes and internal standard in the solvent front zone allows their easy extraction followed by quantitation by HPLC. The exctraction procedure of the solute/s and internal standard can proceed from whole solute frontal zone or its part without lowering in accuracy of quantitative analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Peak broadening in paper chromatography and related techniques : III. Peak broadening in thin-layer chromatography on cellulose powder

    NARCIS (Netherlands)

    Ligny, C.L. de; Remijnse, A.G.

    1968-01-01

    The mechanism of peak broadening in thin-layer chromatography on cellulose powder was investigated by comparing the peak widths obtained in chromatography with those caused only by diffusion in the cellulose powder, for a set of amino acids of widely differing RF values and six kinds of cellulose

  14. Thin-layer chromatography/laser-induced acoustic desorption/electrospray ionization mass spectrometry.

    Science.gov (United States)

    Cheng, Sy-Chyi; Huang, Min-Zong; Shiea, Jentaie

    2009-11-15

    The combination of laser-induced acoustic desorption and electrospray ionization mass spectrometry (LIAD/ESI/MS) can be used to rapidly characterize chemical compounds separated on a thin layer chromatography (TLC) plate. We performed LIAD analysis by irradiating the rear side of an aluminum-based TLC plate with a pulsed infrared (IR) laser. To efficiently generate and transfer acoustic and shock waves to ablate the analyte-containing TLC gels, a glass slide was attached to the rear of the TLC plate and the gap between the glass slide and the TLC plate was filled with a viscous solution (glycerol). Although the diameter of the laser spot created on the rear of the TLC plate was approximately 0.35 mm, the ablated areas on the front sides of the silica gel bed and the C(18) reverse-phase gel bed had diameters of approximately 1.3 and 3 mm, respectively. The ablated analyte molecules were ionized in an ESI plume and then detected by an ion trap mass analyzer. This TLC/LIAD/ESI/MS approach allowed the components in mixtures of dye standards, drug standards, and rosemary essential oil to be separated and rapidly characterized.

  15. Development of optimized mobile phases for protein separation by high performance thin layer chromatography.

    Science.gov (United States)

    Biller, Julia; Morschheuser, Lena; Riedner, Maria; Rohn, Sascha

    2015-10-09

    In recent years, protein chemistry tends inexorably toward the analysis of more complex proteins, proteoforms, and posttranslational protein modifications. Although mass spectrometry developed quite fast correspondingly, sample preparation and separation of these analytes is still a major issue and quite challenging. For many years, electrophoresis seemed to be the method of choice; nonetheless its variance is limited to parameters such as size and charge. When taking a look at traditional (thin-layer) chromatography, further parameters such as polarity and different mobile and stationary phases can be utilized. Further, possibilities of detection are manifold compared to electrophoresis. Similarly, two-dimensional separation can be also performed with thin-layer chromatography (TLC). As the revival of TLC developed enormously in the last decade, it seems to be also an alternative to use high performance thin-layer chromatography (HPTLC) for the separation of proteins. The aim of this study was to establish an HPTLC separation system that allows a separation of protein mixtures over a broad polarity range, or if necessary allowing to modify the separation with only few steps to improve the separation for a specific scope. Several layers and solvent systems have been evaluated to reach a fully utilized and optimized separation system. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Determination of saccharin in pharmaceuticals by high performance thin layer chromatography

    Directory of Open Access Journals (Sweden)

    MIRA CAKAR

    2006-06-01

    Full Text Available A simple, accurate and selective high performance thin layer chromatographic method for the determination of saccharin in pharmaceuticals has been developed. The chromatography was performed on silica-gel 60F254 plates with ethyl acetate–carbon tetrachloride–acetic acid (3 + 4 + 0.5 v/v/v as the mobile phase. The chromatographic zones corresponding to the saccharin spots were scanned in the reflectance/absorbance mode at l= 230 mm. For the standard curves, two series of saccharin sodium salt solutions were prepared: in methanol (solvent 1 and in ethyl acetate–acetic acid (9:1, v/v mixture (solvent 2. A linear calibration relationship was observed within the concentration range from 300 – 1200 ng saccharin sodium salt per spot, correlation coefficients being 0.998 (solvent 1 and 0.995 (solvent 2. The relationship between the peak area and the amount of saccharin sodium salt was evaluated by linear regression analysis. The limits of detection and quantification of saccharin sodium salt were 35 ng and 110 ng per spot (solvent 1, respectively, and 45 ng and 150 ng per spot (solvent 2, respectively. Mean recovery values of 103.5 % (solvent 1 and 102.3 % (solvent 2, and RSD values of 4.42 % (solvent 1 and 2.53 % (solvent 2 were obtained. The proposed method was applied for saccharin determination in two pharmaceutical preparations, effervescent tablets and a carbomer-based gel.

  17. Analysis of Intermediates of Steroid Transformations in Resting Cells by Thin-Layer Chromatography (TLC).

    Science.gov (United States)

    Guevara, Govinda; Perera, Julián; Navarro-Llorens, Juana-María

    2017-01-01

    Thin-layer chromatography (TLC) is a useful and convenient method for the analysis of steroids due to: its simple sample preparation, low time-consuming process, high sensitivity, low equipment investment and capacity to work on many samples simultaneously. Here we describe a TLC easy protocol very useful to analyze steroid molecules derived from a biotransformation carried out in wild-type and mutant resting cells of Rhodococcus ruber strain Chol-4. Following this protocol, we were able to detect the presence or the absence of some well-known intermediates of cholesterol catabolism in Rhodococcus, namely AD, ADD, and 9OHAD.

  18. Dielectric barrier discharge ionization in characterization of organic compounds separated on thin-layer chromatography plates.

    Science.gov (United States)

    Cegłowski, Michał; Smoluch, Marek; Babij, Michał; Gotszalk, Teodor; Silberring, Jerzy; Schroeder, Grzegorz

    2014-01-01

    A new method for on-spot detection and characterization of organic compounds resolved on thin layer chromatography (TLC) plates has been proposed. This method combines TLC with dielectric barrier discharge ionization (DBDI), which produces stable low-temperature plasma. At first, the compounds were separated on TLC plates and then their mass spectra were directly obtained with no additional sample preparation. To obtain good quality spectra the center of a particular TLC spot was heated from the bottom to increase volatility of the compound. MS/MS analyses were also performed to additionally characterize all analytes. The detection limit of proposed method was estimated to be 100 ng/spot of compound.

  19. Identification of common horsetail (Equisetum arvense L.; Equisetaceae) using Thin Layer Chromatography versus DNA barcoding

    DEFF Research Database (Denmark)

    Saslis Lagoudakis, Haris; Bruun-Lund, Sam; Iwanycki, Natalie Eva

    2015-01-01

    The global herbal products market has grown in recent years, making regulation of these products paramount for public healthcare. For instance, the common horsetail (Equisetum arvense L.) is used in numerous herbal products, but it can be adulterated with closely related species, especially E......: a Thin Layer Chromatography approach (TLC-test) included in the European Pharmacopoeia and a DNA barcoding approach, used in recent years to identify material in herbal products. We test the potential of these methods for distinguishing and identifying these species using material from herbarium...

  20. Identification of antibiotic residues in milk by thin-layer chromatography.

    Science.gov (United States)

    Bossuyt, R; Van Renterghem, R; Waes, G

    1976-09-01

    A scheme has been devised that makes it possible to separate and identify, by means of thin-layer chromatography, the 14 different antibiotic resudues in milk which are, besides penicillin, the most widely used in mastitis control: cloxacillin, dihydrostreptomycin, tetracycline, oxytetracycline, chlortetracycline, chloramphenicol, neomycin, novobiocin, bacitracin, erythromycin, oleandomycin, ampicillin, streptomycin and oxacillin. The limits of detectability of the antibiotics studied vary between 0.1 and 3 mug/ml, with the exception of neomycin the minimum detectable concentration of which is 15 mug/ml.

  1. Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography.

    Science.gov (United States)

    Doshi, Gaurav Mahesh; Une, Hemant Devidas

    2016-01-01

    In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida.

  2. [Analysis of pigments from Rhodotorula glutinis by Raman spectroscopy and thin layer chromatography].

    Science.gov (United States)

    Yuan, Yu-feng; Tao, Zhan-hua; Wang, Xue; Li, Yong-qing; Liu, Jun-xian

    2012-03-01

    The pigments from Rhodotorula glutinis were separated by using thin layer chromatography, and the result showed that Rhodotorula glutinis cells could synthesize at least three kinds of pigments, which were beta-carotene, torulene, and torularhodin. The Raman spectra based on the three pigments were acquired, and original spectra were preprocessed by background elimination, baseline correction, and three-point-smoothing, then the averaged spectra from different pigments were investigated, and the result indicated that Raman shift which represents C-C bond was different, and the wave number of beta-carotene demonstrated the largest deviation, finally torulene and torularhodin in Rhodotorula glutinis had more content than beta-carotene. Quantitative analysis of Raman peak height ratio revealed that peak height ratio of pigments showed little difference, which could be used as parameters for further research on living cells, providing reference content of pigments. The above results suggest that Raman spectroscopy combined with thin layer chromatography can be applied to analyze pigments from Rhodotorula glutinis, provides abundant information about pigments, and serves as an effective method to study pigments.

  3. Pixelated scintillator-based compact radio thin layer chromatography scanner for radiopharmaceuticals quality control

    Science.gov (United States)

    Jeon, S. J.; Kim, K. M.; Lim, I.; Song, K.; Kim, J. G.

    2017-11-01

    We evaluated a compact and cost-effective radio thin-layer chromatography (radio-TLC) scanner for the quality control (QC) of radiopharmaceuticals. We adapted a scintillation detector, which is a Gd3Al2Ga3O12 (GAGG:Ce) scintillation crystal array coupled with a photodiode array. The performance of the scintillator array-based radio-TLC was compared with that of a commercial device. We scanned 1 μCi/μL of Tc-99m and F-18 with each device. The difference between the ROI count ratios of the developed and commercial scanners was less than 1.2%. Our scanner is sensitive enough to take measurements for a radiochemical purity test.

  4. Dielectric barrier discharge ionization in characterization of organic compounds separated on thin-layer chromatography plates.

    Directory of Open Access Journals (Sweden)

    Michał Cegłowski

    Full Text Available A new method for on-spot detection and characterization of organic compounds resolved on thin layer chromatography (TLC plates has been proposed. This method combines TLC with dielectric barrier discharge ionization (DBDI, which produces stable low-temperature plasma. At first, the compounds were separated on TLC plates and then their mass spectra were directly obtained with no additional sample preparation. To obtain good quality spectra the center of a particular TLC spot was heated from the bottom to increase volatility of the compound. MS/MS analyses were also performed to additionally characterize all analytes. The detection limit of proposed method was estimated to be 100 ng/spot of compound.

  5. DIFFERENTIATION OF Curcuma longa, Curcuma xanthorrhiza and Zingiber cassumunar BY THIN LAYER CHROMATOGRAPHY FINGERPRINT ANALYSIS

    Directory of Open Access Journals (Sweden)

    Mohamad Rafi

    2011-07-01

    Full Text Available Turmeric (Curcuma longa, java turmeric (Curcuma xanthorrhiza and cassumunar ginger (Zingiber cassumunar are widely used in traditional Indonesian medicine. These three herbs have relatively similar rhizomes colour so it is difficult to be differentiated especially if they are in powder form. A rapid and reliable method, thin layer chromatography (TLC fingerprint, has been developed in order to identify, authenticate and differentiate these three herbs through fingerprint profile of chemical compounds. TLC fingerprints of the three herbs were obtained by visualization of separate zones with visible and UV (254 and 366 nm light. The TLC fingerprint pattern is different each other and showed a specific marker zones respectively. Therefore, TLC fingerprint can be utilized for identification, authentication and differentiation method in quality control of the three herbs tested.

  6. Reversed-phase thin-layer chromatography behavior of aldopentose derivatives

    Directory of Open Access Journals (Sweden)

    Malbaša Radomir V.

    2012-01-01

    Full Text Available Quantitative structure-retention relationships (QSRR have been used to study the chromatographic behavior of some aldopentose. The behavior of aldopentose derivatives was investigated by means of the reversed-phase thin-layer chromatography (RP TLC on the silica gel impregnated with paraffin oil stationary phases. Binary mixtures of methanol-water, acetone-water and dioxane-water were used as mobile phases. Retention factors, RM0, corresponding to zero percent organic modifier in the aqueous mobile phase was determined. Lipophilicity C0 was calculated as the ratio of the intercept and slope values. There was satisfactory correlation between them and log P values calculated using different theoretical procedures. Some of these correlations offer very good predicting models, which are important for a better understanding of the relationships between chemical structure and retention. The study showed that the hydrophobic parameters RM0 and C0 can be used as a measures of lipophilicity of investigated compounds.

  7. High performance thin layer chromatography fingerprint analysis of guava (Psidium guajava) leaves

    Science.gov (United States)

    Astuti, M.; Darusman, L. K.; Rafi, M.

    2017-05-01

    High-performance thin layer chromatography (HPTLC) fingerprint analysis is commonly used for quality control of medicinal plants in term of identification and authentication. In this study, we have been developed HPTLC fingerprint analysis for identification of guava (Psidium guajava) leaves raw material. A mixture of chloroform, acetone, and formic acid in the ratio 10:2:1 was used as the optimum mobile phase in HPTLC silica plate and with 13 bands were detected. As reference marker we chose gallic acid (Rf = 0.21) and catechin (Rf = 0.11). The two compound were detected as pale black bands at 366 nm after derivatization with sulfuric acid 10% v/v (in methanol) reagent. Validation of the method was met within validation criteria, so the developed method could be used for quality control of guava leaves.

  8. A simplified method for rapid quantification of intracellular nucleoside triphosphates by one-dimensional thin-layer chromatography

    DEFF Research Database (Denmark)

    Jendresen, Christian Bille; Kilstrup, Mogens; Martinussen, Jan

    2011-01-01

    -pyrophosphate (PRPP), and inorganic pyrophosphate (PPi) in cell extracts. The method uses one-dimensional thin-layer chromatography (TLC) and radiolabeled biological samples. Nucleotides are resolved at the level of ionic charge in an optimized acidic ammonium formate and chloride solvent, permitting...

  9. Extraction of Nutraceuticals from Spirulina (Blue-Green Alga): A Bioorganic Chemistry Practice Using Thin-layer Chromatography

    Science.gov (United States)

    Herrera Bravo de Laguna, Irma; Toledo Marante, Francisco J.; Luna-Freire, Kristerson R.; Mioso, Roberto

    2015-01-01

    Spirulina is a blue-green alga (cyanobacteria) with high nutritive value. This work provides an innovative and original approach to the consideration of a bioorganic chemistry practice, using Spirulina for the separation of phytochemicals with nutraceutical characteristics via thin-layer chromatography (TLC) plates. The aim is to bring together…

  10. Going Beyond, Going Further. Quantitative Application of Thin-Layer Chromatography in the Analysis of Organic Compounds.

    Science.gov (United States)

    Giuliano, Vincenzo; Rieck, John Paul

    1987-01-01

    Discusses the use of thin-layer chromatography (TLC) in the chemical laboratory as a quantitative method for determining the molecular weights of organic compounds. Describes a simple method which provides an illustration of the importance of polarity on solubility and demonstrates the effectiveness of TLC as a quantitative tool. (TW)

  11. Automated multiple development thin-layer chromatography for separation of opiate alkaloids and derivatives.

    Science.gov (United States)

    Pothier, Jacques; Galand, Nicole

    2005-07-08

    There are three types of opiate alkaloids. First, the poppy alkaloids: morphine, codeine, thebaine, noscapine and papaverine; then, the semi-synthetic and synthetic derivatives used in therapy as antitussives and analgesics, such as pholcodine, ethylmorphine and dextromethorphan; at last narcotic compounds, diacetylmorphine (heroin) and opiates employed as substitutes in treatment of addiction: buprenorphine and methadone. For classical thin-layer chromatography (TLC) of opium alkaloids, it is necessary to use complex eluents with strong alkaline substances to obtain a clean separation between morphinan and isoquinoline compounds. This study purposes the planar chromatographic analysis of these substances by the automated multiple development (AMD) compared with results obtained by classical TLC method. The aim of this work was to achieve the best separation of these opiate alkaloids and derivatives by this modern technique of planar chromatography. The AMD system provided a clean separation for each of three opiates groups studied and the best results have been obtained with universal gradient: methanol 100, methanol-dichloromethane 50/50, dichloromethane 100, dichloromethane 100, hexane 100 for opium alkaloids and with gradient A: 5% of 28% ammonia in methanol 100, acetone 100, acetone 100, ethyl acetate-dichloromethane 50/50, dichloromethane 100 for antitussives and substitutes. Two reagents were used for the detection of alkaloids by spraying: Dragendorff and iodoplatinate reagents. The detection limits with these two reagents were 1 microg for ethylmorphine, thebaine, papaverine, codeine, and 2 microg for morphine and noscapine and other alkaloids.

  12. Hydrocarbon group-type analysis by thin layer chromatography and scanning densitometry

    Energy Technology Data Exchange (ETDEWEB)

    Membrado, L.; Cebolla, V.L.; Matt, M.; Galvez, E.M.; Domingo, M.P.; Vela, J.; Beregovtsova, N. [CSIC, Zaragoza (Spain)

    2002-07-01

    Hydrocarbon group-type analysis (HGTA) is a common technique for characterization of complex mixtures derived from raw materials such as coal, petroleum, or biomass. In these and other, related, samples, trying to achieve extensive separation of all the components would be very difficult at least, and most of the relevant properties of the samples can be related to the amounts of the different types of hydrocarbon. Groups of interest depend mainly on the nature of the sample, and some kind of liquid chromatography is usually involved in the most common HGTA methods. Thin-layer chromatography (TLC) can nowadays usually be used instead of HPLC, resulting in several advantages in terms of speed, cost, and general convenience. Detection and quantification of the different peaks might involve the use of special equipment, e.g. in TLC-flame ionization detection (FID) methods, although it can also be accomplished by means of UV and fluorescence scanning densitometry. This paper describes a series of TLC-based HGTA methods developed for coal-, biomass-, and petroleum-derived products that give a reasonably general overview of the possibilities of TLC applied to HGTA.

  13. Indirect fluorometric detection techniques on thin layer chromatography and effect of ultrasound on gel electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Yinfa, Ma.

    1990-12-10

    Thin-layer chromatography (TLC) is a broadly applicable separation technique. It offers many advantages over high performance liquid chromatography (HPLC), such as easily adapted for two-dimensional separation, for whole-column'' detection and for handling multiple samples, etc. However, due to its draggy development of detection techniques comparing with HPLC, TLC has not received the attention it deserves. Therefore, exploring new detection techniques is very important to the development of TLC. It is the principal of this dissertation to present a new detection method for TLC -- indirect fluorometric detection method. This detection technique is universal sensitive, nondestructive, and simple. This will be described in detail from Sections 1 through Section 5. Section 1 and 3 describe the indirect fluorometric detection of anions and nonelectrolytes in TLC. In Section 2, a detection method for cations based on fluorescence quenching of ethidium bromide is presented. In Section 4, a simple and interesting TLC experiment is designed, three different fluorescence detection principles are used for the determination of caffeine, saccharin and sodium benzoate in beverages. A laser-based indirect fluorometric detection technique in TLC is developed in Section 5. Section 6 is totally different from Sections 1 through 5. An ultrasonic effect on the separation of DNA fragments in agarose gel electrophoresis is investigated. 262 refs.

  14. Analyzing salvia divinorum and its active ingredient salvinorin a utilizing thin layer chromatography and gas chromatography/mass spectrometry.

    Science.gov (United States)

    Jermain, John D; Evans, Hiram K

    2009-05-01

    In recent years, Salvia divinorum has become a major focus by state legislatures throughout the United States looking to prohibit the sale of the psychoactive plant. After researching testing procedures presented in the literature and those employed by crime laboratories throughout the country, it was decided that thin layer chromatography (TLC) and gas chromatography/mass spectrometry (GC/MS) were the methods to use to analyze plant material for salvinorin A. With TLC, salvinorin A was detected from extracted plant material and was easily distinguishable from 13 other Salvia species as well as Cannabis sativa L. (marijuana). When using GC/MS, salvinorin A was best extracted from plant material with chloroform at ambient temperature when using a nonpolar solvent and acetone at ambient temperature when using a polar solvent. By utilizing these techniques, criminalists are now able to confirm the presence of salvinorin A in a submitted plant material suspected to be Salvia divinorum.

  15. Identification of common horsetail (Equisetum arvense L.; Equisetaceae) using Thin Layer Chromatography versus DNA barcoding.

    Science.gov (United States)

    Saslis-Lagoudakis, C Haris; Bruun-Lund, Sam; Iwanycki, Natalie E; Seberg, Ole; Petersen, Gitte; Jäger, Anna K; Rønsted, Nina

    2015-07-13

    The global herbal products market has grown in recent years, making regulation of these products paramount for public healthcare. For instance, the common horsetail (Equisetum arvense L.) is used in numerous herbal products, but it can be adulterated with closely related species, especially E. palustre L. that can produce toxic alkaloids. As morphology-based identification is often difficult or impossible, the identification of processed material can be aided by molecular techniques. In this study, we explore two molecular identification techniques as methods of testing the purity of these products: a Thin Layer Chromatography approach (TLC-test) included in the European Pharmacopoeia and a DNA barcoding approach, used in recent years to identify material in herbal products. We test the potential of these methods for distinguishing and identifying these species using material from herbarium collections and commercial herbal products. We find that both methods can discriminate between the two species and positively identify E. arvense. The TLC-test is more cost- and time-efficient, but DNA barcoding is more powerful in determining the identity of adulterant species. Our study shows that, although DNA barcoding presents certain advantages, other established laboratory methods can perform as well or even better in confirming species' identity in herbal products.

  16. Discrimination of reactively-dyed cotton fibres with thin layer chromatography and UV microspectrophotometry.

    Science.gov (United States)

    De Wael, K; Van Dijck, K; Gason, F

    2015-12-01

    Reactively-dyed black, navy blue and medium red cotton samples showing metamerism under fluorescent tube illumination were examined. Optical microscopy (bright field, polarization and fluorescence microscopy) was used, followed by microspectrometry in the visible range (MSP Vis), to differentiate the samples in each block of colours. Additionally, the non-discriminated samples were subjected both to microspectrophotometry in the UV-range (MSP UV) and to enzymatic digestion followed by high performance thin layer chromatography (HPTLC) on the digests. While it was found that both methods may potentially result in higher discrimination, preparation of reactively-dyed cotton for HPTLC was found to be a very tedious and time-consuming step and HPTLC only led to a better discrimination than MSP UV for the red cotton samples. The results suggest that in order to increase the discrimination for reactively-dyed cotton fibres, measurement of the UV absorption spectrum (MSP UV) is preferred over HPTLC. Copyright © 2015 The Chartered Society of Forensic Sciences. Published by Elsevier Ireland Ltd. All rights reserved.

  17. Thin layer chromatography of p-aminophenol in urine after mixed exposure to aniline and toluene.

    Science.gov (United States)

    Bieniek, G; Karmańska, K; Wilczok, T

    1984-01-01

    A simple method of evaluating p-aminophenol in the urine of people exposed simultaneously to aniline and toluene relies on separating p-aminophenol from hippuric acid and other physiological components of the urine by thin layer chromatography. The adsorbents and developing system have been thus fixed to make possible the separation of p-aminophenol from hippuric acid, urea, and creatinine and their quantitative determination. This method also makes possible the determination of p-aminophenol in urine in the presence of hippuric acid. Hippuric acid is a physiological component of urine and also the metabolite of toluene, so the determination of p-aminophenol is possible also after simultaneous exposure to both compounds: aniline and toluene. At the same time the concentrations of urea and creatinine as additional factors may be determined. The limit of detection of the method is: 5 micrograms/ml for p-aminophenol, 9 micrograms/ml for hippuric acid, 8 micrograms/ml for urea, and 6 micrograms/ml for creatinine. PMID:6722055

  18. HPTLC-aptastaining - Innovative protein detection system for high-performance thin-layer chromatography

    Science.gov (United States)

    Morschheuser, Lena; Wessels, Hauke; Pille, Christina; Fischer, Judith; Hünniger, Tim; Fischer, Markus; Paschke-Kratzin, Angelika; Rohn, Sascha

    2016-05-01

    Protein analysis using high-performance thin-layer chromatography (HPTLC) is not commonly used but can complement traditional electrophoretic and mass spectrometric approaches in a unique way. Due to various detection protocols and possibilities for hyphenation, HPTLC protein analysis is a promising alternative for e.g., investigating posttranslational modifications. This study exemplarily focused on the investigation of lysozyme, an enzyme which is occurring in eggs and technologically added to foods and beverages such as wine. The detection of lysozyme is mandatory, as it might trigger allergenic reactions in sensitive individuals. To underline the advantages of HPTLC in protein analysis, the development of innovative, highly specific staining protocols leads to improved sensitivity for protein detection on HPTLC plates in comparison to universal protein derivatization reagents. This study aimed at developing a detection methodology for HPTLC separated proteins using aptamers. Due to their affinity and specificity towards a wide range of targets, an aptamer based staining procedure on HPTLC (HPTLC-aptastaining) will enable manifold analytical possibilities. Besides the proof of its applicability for the very first time, (i) aptamer-based staining of proteins is applicable on different stationary phase materials and (ii) furthermore, it can be used as an approach for a semi-quantitative estimation of protein concentrations.

  19. Radiotracer binding to brain microsomes determined by thin-layer chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Zamora, P.O.; Stratesteffan, M.; Guhlke, S.; Sass, K.S.; Cardillo, A.; Bender, H.; Biersack, H.J

    1996-01-01

    A thin-layer chromatography (TLC) assay was developed to monitor the interaction of radiotracers with brain microsomes. Murine brain microsomes were coated onto a zone of a TLC strip, the unreacted sites blocked with gelatin, and the radiotracers chromatographed over the microsomes. Radiotracers bound to the microsomes and were separated from the unreacted materials which migrated at or near the solvent front. Up to 80% of the applied radioactivity bound to the brain microsomes when using {sup 99m}Tc-(d,l) hexamethyl-propyleneamine oxime (HMPAO) and {sup 123}I-(S)-2-hydroxy-3-iodo-6-methoxy-N-[(1-ethyl-2-pyrrolidinyl)methyl]- benzamide ({sup 123}I-IBZM) as tracers. On the other hand, the presumptive negative control materials p-I-15-phenyl-pentadecanoic acid-{sup 123}I ({sup I}I-IPPA) and {sup 99m}Tc-mercapto-acetyl triglycine (MAG3) bound poorly (7% and 4%, respectively). {sup 99m}Tc-ethyl cysteinate dimer (ECD) interacted poorly (9.9%), a result thought to be consistent with its known inability to be metabolized by nonprimate brain tissue. Radiolabeled octreotide analogues (radiolabeled with {sup 111}In, I-131 or {sup 99m}Tc) also bound, and the binding could be reduced by excess unlabeled octreotide. Also, chemical modification by acylation of Lys{sup 5} in {sup 111}In-labeled octreotide led to decreased binding (approximately 70%) compared to the original radiotracer. Chromatography of the various radiotracers over TLC strips coated only with gelatin was used to monitor nonspecific binding and was low and frequently below 5%. This technique does not require wash steps or centrifugation, and assays are rapidly completed. The assay could be useful in monitoring the interaction of radiotracers with brain microsomes and in evaluating and developing new radiotracers.

  20. Detection of Griseofulvin and Dechlorogriseofulvin by Thin-Layer Chromatography and Gas-Liquid Chromatography

    Science.gov (United States)

    Cole, R. J.; Kirksey, J. W.; Holaday, C. E.

    1970-01-01

    A rapid and accurate method is described for the determination of griseofulvin and dechlorogriseofulvin extracted from Penicillium urticae with chloroform. Thinlayer chromatography was used to tentatively identify griseofulvin or dechlorogriseofulvin, or both. Two gas-liquid chromatographic systems provided additional qualitative information and simultaneous quantitation of the individual compounds. PMID:5415206

  1. The phytochemical screening and thin layer chromatography results of Jatropha gossypiifolia seeds

    Directory of Open Access Journals (Sweden)

    Anis Nurwidayati

    2013-05-01

    , the intermediary for schistosomiasis is widespread in this region. Eradication has been done by spraying chemical molluscicides. This study aimed to identify the class of chemical compounds in the methanol extract of red castor seed.Methods: The study was conducted in May 2009. Red castor seeds were collected from Palu, Central Sulawesi. Red castor seeds extraction was done by percolation method using methanol solvent. Phytochemical screening test was performed with a tube to detect the compound in red castor bean extract. Screening was followed by thin layer chromatography testing to ensure the screening results of the test tube.Results:Extracts that was produced from 500 grams of red castor dry seed powder with 2500 ml of methanol solvent was 250 ml thick reddish brown fluid. Phytochemical screening with a test tube showed positive results of alkaloid by the formation of deposits in Meyer test, Wagner test, and Dragendorff test. Screening the methanol extracts of red castor seed also showed positive results on saponins by foam test and LiebermanBurchard test. Positive results on Killiani Keller tests and Kedde test suggests that red castor bean extract contains cardenoline and bufadienol. Thin-layer chromatography analysis showed that the red castor bean extract is positive for terpenes with the formation of spots on the silica gel plate when terpenes was sprayed (cerium sulfate reagent. Conclusion: Chemical components contained in the methanol extract of red castor beans consisted of alkaloids, saponins, cardenolin, bufadienol, and terpenes. (Health Science Indones 2012;2:xx-xxKeywords: schistosomiasis, Jatropha gossypifolia, chemical compound

  2. Validation of a thin-layer chromatography/densitometry method for the characterization of invertase activity.

    Science.gov (United States)

    Ferey, Justine; Da Silva, David; Bravo-Veyrat, Sophie; Lafite, Pierre; Daniellou, Richard; Maunit, Benoît

    2016-12-16

    This paper presents a kinetic study of invertase, a specific fructofuranosidase cloned from the Leishmania major genome. The kinetic parameters of the β-d-fructofuranosidase from Leishmania major (BfrA) were determined using Thin-Layer Chromatography (TLC) and UV-densitometry (TLC@UV) specifically developed for the separation and detection of three carbohydrates namely sucrose, glucose and fructose. Separation was performed on TLC silica gel 60 F254 plates impregnated with sodium bisulphate and citrate and heated prior to development. This fast and easy separation was performed with two successive developments using ACN/H2O 80/20 (v/v) as mobile phase. Sensitive and repeatable derivatization of sugars was achieved by dipping the plates in a solution of 4-aminobenzoic acid. Quantification was performed by UV-detection. The method was validated according to ICH guidelines Q2(R1) in terms of specificity, limits of detection and quantification, precision and robustness (with n=3 replicates and CV ≤10%). The characterization of BfrA reaction kinetic was performed by monitoring the accumulation of either glucose or fructose detected by TLC@UV. Hydrolysis of sucrose was described by the Michaelis-Menten kinetic parameters (KM; Vmax) respectively equal to 63.09±7.590mM; 0.037±0.00094mM/min using glucose production and 83.01±14.39mM; 0.031±0.0021mM/min monitoring fructose. Hydrolyses of three alternative substrates, raffinose, stachyose and inulin, were also compared and the regiospecificity of the reaction was characterized. This TLC@UV method is shown to be suitable for the refined kinetic analysis of different reactions related to the hydrolysis of sugars. Copyright © 2016. Published by Elsevier B.V.

  3. Thin-layer chromatography analysis and scavenging activity of marigold (Calendula officinalis L extracts

    Directory of Open Access Journals (Sweden)

    Ćetković Gordana S.

    2003-01-01

    Full Text Available The methanol, petroleum ether, chloroform, ethyl acetate, n-butanol and water extracts were obtained by extraction of marigold flower (Calendula officinalis L. The content of total phenolic compounds, determined by UV spectrophotometric method using the Folin-Ciocalteu reagent, was 15.12 mg/g. The content of total flavonoids, determined by UV spectrophotometric method according to Markham, was 5.13 mg/g. Qualitative determination of phenolic compounds in the extracts was performed by one- and two-dimensional thin-layer chromatography (TLC procedures. The results of one- and two-dimensional TLC analyses showed that different flavonoids and phenolic acids were present in the investigated extracts. The greatest number of flavonoids (rutin, quercetin and some unidentified flavonoid glycosides and phenolic acids (chlorogenic, caffeic, coumaric and vanillic acid were deteminated in methanol extract. The influence of marigold extracts, in concentration range 0.6-1.2 mg/mL, on 2,2’-diphenyl-1-picrylhydrazyl (DPPH free radicals was investigated by electron spin resonance (ESR spectroscopy. All extracts showed scavenging activity (SA in the following order: ethyl acetate > n-butanol > methanol > water > chloroform > petroleum ether. The SA increased with increasing concentration of extracts. The ethyl acetate and n-butanol extracts exibited the most significant SA. These extracts in concentration of 1.2 mg/mL eliminated completely DPPH radicals. The lowest SA had chloroform and petroleum ether extracts (in concentration of 0.6 mg/mL SA=0%. The SA of marigold extracts is attributed to its hydrogen-donating ability and scavenging effect.

  4. High Performance Thin Layer Chromatography method for analysis of 3,4-methylenedioxymethamphetamine in seized tablets

    Directory of Open Access Journals (Sweden)

    Boris E. Duffau

    2015-12-01

    Full Text Available Context: Consumption of synthetic drugs had increased in recent years, used as a recreational drug by young people who presume that consumption of this drug is harmless for health; however clinical studies have shown that this stimulant and its metabolites are toxic. Due to these reasons, chemical analysis of this illicit drug is crucial from the points of view of occupational medicine, toxicology, and law enforcement with the aim of pursuit the traffic of illegal drug. Aims: Implement and fully validate a rapid and simple method for detection and quantitation of MDMA by High-Performance Thin Layer Chromatography in seized samples. Methods: With the implemented method was analyzed 12 positive samples seized by Chilean police, to found the concentration of MDMA in ecstasy tablets. Results: The method was fully validated, the linearity of the method was evaluated by the calibration curve between 51.0 – 510.0 µg/band (R2 0.9977; limit of detection was 12.1 µg per band, and limit of quantitation was 36.8 µg per band. The precision of the method (RSD was lower than 5.0%. Accuracy was evaluated by determination of the percentage of MDMA recovered by the assay (99.13%, and relative Uncertainty was 6.66%. With this method, it was analyzed real seized samples of MDMA, results showed that all samples contained MDMA and concentration was between 18.15 – 59.84 % w/w. Conclusions: The method is selective, sensitive, and specific, with possible application in forensic analysis. To the best of our knowledge, this is the first report about concentration of MDMA in ecstasy pills in Chile.

  5. Employment of High-Performance Thin-Layer Chromatography for the Quantification of Oleuropein in Olive Leaves and the Selection of a Suitable Solvent System for Its Isolation with Centrifugal Partition Chromatography.

    Science.gov (United States)

    Boka, Vasiliki-Ioanna; Argyropoulou, Aikaterini; Gikas, Evangelos; Angelis, Apostolis; Aligiannis, Nektarios; Skaltsounis, Alexios-Leandros

    2015-11-01

    A high-performance thin-layer chromatographic methodology was developed and validated for the isolation and quantitative determination of oleuropein in two extracts of Olea europaea leaves. OLE_A was a crude acetone extract, while OLE_AA was its defatted residue. Initially, high-performance thin-layer chromatography was employed for the purification process of oleuropein with fast centrifugal partition chromatography, replacing high-performance liquid-chromatography, in the stage of the determination of the distribution coefficient and the retention volume. A densitometric method was developed for the determination of the distribution coefficients, KC = CS/CM. The total concentrations of the target compound in the stationary phase (CS) and in the mobile phase (CM) were calculated by the area measured in the high-performance thin-layer chromatogram. The estimated Kc was also used for the calculation of the retention volume, VR, with a chromatographic retention equation. The obtained data were successfully applied for the purification of oleuropein and the experimental results confirmed the theoretical predictions, indicating that high-performance thin-layer chromatography could be an important counterpart in the phytochemical study of natural products. The isolated oleuropein (purity > 95%) was subsequently used for the estimation of its content in each extract with a simple, sensitive and accurate high-performance thin-layer chromatography method. The best fit calibration curve from 1.0 µg/track to 6.0 µg/track of oleuropein was polynomial and the quantification was achieved by UV detection at λ 240 nm. The method was validated giving rise to an efficient and high-throughput procedure, with the relative standard deviation % of repeatability and intermediate precision not exceeding 4.9% and accuracy between 92% and 98% (recovery rates). Moreover, the method was validated for robustness, limit of quantitation, and limit of detection. The amount of oleuropein for

  6. Development and validation of a high-performance thin layer chromatography method for the determination of cholesterol concentration

    Directory of Open Access Journals (Sweden)

    Jinu John

    2015-06-01

    Full Text Available An accurate, sensitive, precise, reliable, and quick method for the determination of cholesterol content by high-performance thin layer chromatography is developed. In this method, aluminum-backed precoated silica gel 60 F254 plates were used as the stationary phase and the samples were sprayed with the help of CAMAG sample applicator Linomat 5. The chromatogram was developed with the mobile phase consisting of chloroform:methanol (9.5:0.5, v/v. The samples were detected using CAMAG Scanner 4 and evaluated using the method developed on winCATS software. Densitometric analysis of cholesterol was performed in absorbance mode at 200 nm. In this solvent system, cholesterol gave a compact spot with an Rf value of 0.63 ± 0.03. The linear regression analysis of data for the calibration curve showed good linearity over a concentration range of 2–7 μg/spot with a regression value of 0.99933 and standard deviation of 1.44%. The limit of detection and limit of quantification were found to be 100 ng/spot and 500 ng/spot, respectively. Using the developed method, the concentration of cholesterol in the saponified and unsaponified egg yolk sample was determined. This method was found to be reproducible and can even be used for samples containing complex matrices.

  7. Analysis of low active-pharmaceutical-ingredient signal drugs based on thin layer chromatography and surface-enhanced Raman spectroscopy.

    Science.gov (United States)

    Li, Xiao; Chen, Hui; Zhu, Qingxia; Liu, Yan; Lu, Feng

    2016-11-30

    Active pharmaceutical ingredients (API) embedded in the excipients of the formula can usually be unravelled by normal Raman spectroscopy (NRS). However, more and more drugs with low API content and/or low Raman scattering coefficient were insensitive to NRS analysis, which was for the first time defined as Low API-Signal Drugs (LASIDs) in this paper. The NRS spectra of these LASIDs were similar to their dominant excipients' profiles, such as lactose, starch, microcrystalline cellulose (MCC), etc., and were classified into three types as such. 21 out of 100 kinds of drugs were screened as LASIDs and characterized further by Raman microscopic mapping. Accordingly, we proposed a tailored solution to the qualitation and quantitation problem of these LASIDs, using surface-enhanced Raman spectroscopic (SERS) detection on the thin layer chromatographic (TLC) plate both in situ and after-separation. Experimental conditions and parameters including TLC support matrix, SERS substrate, detection mode, similarity threshold, internal standard, etc., were optimized. All LASIDs were satisfactorily identified and the quantitation results agreed well with those of high performance liquid chromatography (HPLC). For some structural analogues of LASIDs, although they presented highly similar SERS spectra and were tough to distinguish even with Raman microscopic mapping, they could be successfully discriminated from each other by coupling SERS (with portable Raman spectrometer) with TLC. These results demonstrated that the proposed solution could be employed to detect the LASIDs with high accuracy and cost-effectiveness. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Thin-layer chromatography with UV-scanning detection for quantitative analysis of coal-derived products

    Energy Technology Data Exchange (ETDEWEB)

    Vela, J.; Cebolla, V.L.; Membrado, L.; Ferrando, A.C. [University of Zaragoza, Zaragoza (Spain). Dept. of Analytical Chemistry

    1998-07-01

    Quantitative analysis of hydrocarbon groups (HGTA) is important in the characterization of products derived from coal conversion. The heaviest products are usually analyzed by thin-layer chromatography with flame-ionization detection (TLC-FID). TLC with ultraviolet (UV) scanning densitometry was investigated as an alternative to TLC-FID for the rapid determination of aromatic, polar, and noneluted compounds in coal-derived products. The results obtained show that TLC-UV is adequate in terms of speed, repeatability, and quantitative analysis, and furnishes results similar to those obtained by TLC-FID. Preparative TLC enables isolation of fractions suitable for preparative purposes and is less time-consuming (hours rather than days) than LC methods. Rapid calibration of TLC-UV is possible by use of fractions isolated by preparative TLC (derived from the actual fossil fuels to be analyzed) as external standards. A method of fast internal calibration has been tested for hydrocarbon group-type analysis. Direct acquisition of UV spectra from the separated peaks can be used to determine whether this method of calibration is applicable to the sample.

  9. Quantitative Thin-Layer Chromatography/Mass Spectrometry Analysis of Caffeine Using a Surface Sampling Probe Electrospray Ionization Tandem Mass Spectrometry System

    Energy Technology Data Exchange (ETDEWEB)

    Ford, Michael J [ORNL; Deibel, Michael A. [Earlham College; Tomkins, Bruce A [ORNL; Van Berkel, Gary J [ORNL

    2005-01-01

    Quantitative determination of caffeine on reversed-phase C8 thin-layer chromatography plates using a surface sampling electrospray ionization system with tandem mass spectrometry detection is reported. The thin-layer chromatography/electrospray tandem mass spectrometry method employed a deuterium-labeled caffeine internal standard and selected reaction monitoring detection. Up to nine parallel caffeine bands on a single plate were sampled in a single surface scanning experiment requiring 35 min at a surface scan rate of 44 {mu}m/s. A reversed-phase HPLC/UV caffeine assay was developed in parallel to assess the mass spectrometry method performance. Limits of detection for the HPLC/UV and thin-layer chromatography/electrospray tandem mass spectrometry methods determined from the calibration curve statistics were 0.20 ng injected (0.50 {mu}L) and 1.0 ng spotted on the plate, respectively. Spike recoveries with standards and real samples ranged between 97 and 106% for both methods. The caffeine content of three diet soft drinks (Diet Coke, Diet Cherry Coke, Diet Pepsi) and three diet sport drinks (Diet Turbo Tea, Speed Stack Grape, Speed Stack Fruit Punch) was measured. The HPLC/UV and mass spectrometry determinations were in general agreement, and these values were consistent with the quoted values for two of the three diet colas. In the case of Diet Cherry Coke and the diet sports drinks, the determined caffeine amounts using both methods were consistently higher (by 8% or more) than the literature values.

  10. Simple Identification of the Neutral Chlorinated Auxin in Pea by Thin Layer Chromatography

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen

    1980-01-01

    One of the neutral chlorinated auxins of immature pea seeds was readily identified by thin layer procedures simple enough to serve in student's laboratory courses. 4-Chloroindole-3-acetic acid methyl ester was extracted from 50 g of commercial, frozen peas by either water or acetone, concentrated...

  11. Nevirapine concentrations in saliva measured by thin layer chromatography and self-reported adherence in patients on antiretroviral therapy at kilimanjaro christian medical centre, Tanzania

    NARCIS (Netherlands)

    George, L.; Muro, E.P.; Ndaro, A.; Dolmans, W.M.; Burger, D.M.; Kisanga, E.R.

    2014-01-01

    BACKGROUND: Thin layer chromatography (TLC) can be used to perform therapeutic drug monitoring in resource-limited settings, where more expensive analytical methods, such as high-performance liquid chromatography or liquid chromatography-mass spectrometry, are not feasible. OBJECTIVES: The aim of

  12. Development and validation of High-performance Thin-layer Chromatography Method for Simultaneous Determination of Polyphenolic Compounds in Medicinal Plants

    Science.gov (United States)

    Jayachandran Nair, C. V.; Ahamad, Sayeed; Khan, Washim; Anjum, Varisha; Mathur, Rajani

    2017-01-01

    Context: Quantitative standardization of plant-based products is challenging albeit essential to maintain their quality. Aims: This study aims to develop and validate high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination of rutin (Ru), quercetin (Qu), and gallic acid (Ga) from Psidium guajava Linn. (PG) and Aegle marmelos (L.) Correa. (AM) and correlate with antioxidant activity. Materials and Methods: The stock solution (1 mg/mL) of standard Ru, Qu, and Ga in methanol: Water (1:1) was serially diluted and spotted (5 μL) on slica gel 60 F254 thin-layer chromatography plates. Toluene: Ethyl acetate: Formic acid: Methanol (3:4:0.8:0.7, v/v/v) was selected as mobile phase for analysis at 254 nm. Hydroalcoholic (1:1) extracts of leaves of PG and AM were fractionated and similarly analyzed. Antioxidant activity was also determined using 2, 2-diphenyl-1-picrylhydrazyl assay. Results: The developed method was robust and resolved Ru, Qu, and Ga at Rf 0.08 ± 0.02, 0.76 ± 0.01, and 0.63 ± 0.02, respectively. The intra-day, interday precision, and interanalyst were Psidium guajava; Qu: Quercetin; Ru: Rutin. PMID:29333046

  13. Separation of Berberine Hydrochloride and Tetrahydropalmatine and Their Quantitative Analysis with Thin Layer Chromatography Involved with Ionic Liquids

    Directory of Open Access Journals (Sweden)

    Jing Lu

    2015-01-01

    Full Text Available [BMIM]OH was used in mobile and stationary phase of thin layer chromatography (TLC to analyze berberine hydrochloride and tetrahydropalmatine for the first time. Supported imidazole ionic liquid with hydroxide ion on silica gel (SiO2·Im+·OH− was synthesized through simple procedure and characterized by Fourier transform infrared spectroscopy (FT-IR, elemental analysis, and scanning electron microscope (SEM. Moreover, on the plates prepared by SiO2·Im+·OH−, the contents of the above alkaloids in the Chinese patent medicine (CPM of “Stomacheasy” capsule were successfully determined by TLC scanner. The key conditions and chromatographic behaviors were also investigated in detail. According to similar ways, ionic liquids (ILs also can be used in other planar chromatographies in two modes. This study is expected to be helpful in expanding the application of IL and its bonded silica gel in TLC separation field.

  14. Thin-layer chromatography with flame ionization detection in the characterization of pitches

    Energy Technology Data Exchange (ETDEWEB)

    Cebolla, V.L.; Membrado, L.; Vela, J. [Instituto de Carboquimica, Zaragoza (Spain)] [and others

    1995-12-31

    TLC-FID is a rapid, quality-control oriented technique which joins the advantages of Thin-Layer (TLC) with the possibility of quantification of the separated peaks using a Flame Ionization Detector (FID). In the case of heavy fossil fuels, group-type analysis can be achieved with the possibility of a direct quantification of heavy/polar groups, without any preseparation, and in short analysis times with regard to the current techniques. However, although TLC-FID has been used since the eighties in many fields of Chemistry, results were demonstrated to depend on the technique (analytical system plus methodology) used. This work intends to analyze the fundamental parameters involved in TLC-FID technique using adequate technology and methodology, and to lay the groundwork for a correct group-type characterization of pitches.

  15. Development and validation of high-performance liquid chromatography and high-performance thin-layer chromatography methods for the quantification of khellin in Ammi visnaga seed.

    Science.gov (United States)

    Kamal, Abid; Khan, Washim; Ahmad, Sayeed; Ahmad, F J; Saleem, Kishwar

    2015-01-01

    The present study was used to design simple, accurate and sensitive reversed phase-high-performance liquid chromatography RP-HPLC and high-performance thin-layer chromatography (HPTLC) methods for the development of quantification of khellin present in the seeds of Ammi visnaga. RP-HPLC analysis was performed on a C18 column with methanol: Water (75: 25, v/v) as a mobile phase. The HPTLC method involved densitometric evaluation of khellin after resolving it on silica gel plate using ethyl acetate: Toluene: Formic acid (5.5:4.0:0.5, v/v/v) as a mobile phase. The developed HPLC and HPTLC methods were validated for precision (interday, intraday and intersystem), robustness and accuracy, limit of detection and limit of quantification. The relationship between the concentration of standard solutions and the peak response was linear in both HPLC and HPTLC methods with the concentration range of 10-80 μg/mL in HPLC and 25-1,000 ng/spot in HPTLC for khellin. The % relative standard deviation values for method precision was found to be 0.63-1.97%, 0.62-2.05% in HPLC and HPTLC for khellin respectively. Accuracy of the method was checked by recovery studies conducted at three different concentration levels and the average percentage recovery was found to be 100.53% in HPLC and 100.08% in HPTLC for khellin. The developed HPLC and HPTLC methods for the quantification of khellin were found simple, precise, specific, sensitive and accurate which can be used for routine analysis and quality control of A. visnaga and several formulations containing it as an ingredient.

  16. Monitoring of monooctanoyl phosphatidylcholine synthesis by enzymatic acidolysis between soybean phosphatidylcholine and caprylic acid by thin-layer chromatography with a flame ionization detector

    DEFF Research Database (Denmark)

    Vikbjerg, Anders Falk; Mu, Huiling; Xu, Xuebing

    2005-01-01

    Thin-layer chromatography with flame ionization detector (TLC-FID) method was used for monitoring the production of structured phospholipids (ML-type: L-long chain fatty acids; M-medium chain fatty acids) by enzyme-catalyzed acidolysis between soybean phosphatidylcholine (PC) and caprylic acid....... It was found that the structured PC fractionated into 2-3 distinct bands on both plate thin layer chromatography (TLC) and Chromarod TLC. These 3 bands represented PC of LL-type, ML-type and MM-type, respectively. The TLC-FID method was applied in the present study to examine the influence of enzyme dosage...

  17. [Resolution of clenbuterol hydrochloride enantiomers by thin-layer chromatography on silica gel impregnated with beta-cyclodextrin].

    Science.gov (United States)

    Yu, Jingang; Huang, Kelong; Jiao, Feipeng; Peng, Xiahui

    2005-07-01

    The resolution of clenbuterol hydrochloride enantiomers was achieved by thin-layer chromatography on silica gel GF254 plates impregnated w ith beta-cyclodextrin. The effect of stereoselective auxiliary (acetonitrile and alcohol) was investigated. Resolution of clenbuterol hydrochloride enantiomers could be attained by using alcohols of butanol, 2-butanol or tert-butanol together with acetonitrile as developing solvent. The optimal conditions of resolution were determined as follows: a plate prepared with 15.00 g silica gel GF254 impregnated with 1.00 g beta-cyclodextrin, acetonitrile-2-butanol (20:80, v/v) as developing solvent and developed at room temperature. Under these conditions, Rf of the two isomers of clenbuterol hydrochloride enantiomers were 0.34 and 0.72 respectively. The resolution was 4.09 with baseline separation and the spots in chromatogram were almost of the same size.

  18. Immunological analysis of food proteins using high-performance thin-layer chromatography-immunostaining.

    Science.gov (United States)

    Morschheuser, Lena; Mink, Kathrin; Horst, Ramona; Kallinich, Constanze; Rohn, Sascha

    2017-12-01

    The chromatographic analysis of intact proteins is still challenging, especially when biological functions as antigenicity of proteins or peptides are in the focus. Traditional immunoassays provide information about the entirety of antigenic proteins/peptides, e.g., in ELISA assays. On the other hand, when focusing on the investigation of (cross) reactivity of antibodies, Western blot following gel-electrophoresis represents the method of choice. However, gel-electrophoresis is limited by the molecular weight and therefore, not suitable for peptides ≤3kDa or proteins ≥250kDa. Furthermore, for gaining detailed information about the protein sequence (e.g., via mass spectrometric analysis), a so called in-gel digest needs to be performed following electrophoretic separation and is therefore elaborate and accompanied by a significant loss of structural, and even more severe, conformational information. Here, protein analysis using HPTLC seems to be a promising alternative due to the high level of variability regarding the chromatographic system (multiple mobile and stationary phases, even mixed) and manifold detection as well as hyphenation possibilities. This study exemplarily focused on the immunological investigation of proteins in milk following thin-layer chromatographic separation. The detection of these antigens is mandatory, as they might trigger allergenic reactions in sensitized people. Besides the proof of its applicability on different stationary phase materials, the newly developed immunoassay can be used as an approach for semi-quantitative estimation of antigenic proteins. In addition to the analysis of intact food allergens, also analyzing peptides thereof is worth considering which can be realized using HPTLC-immunostaining as well. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Effect-directed analysis via hyphenated high-performance thin-layer chromatography for bioanalytical profiling of sunflower leaves.

    Science.gov (United States)

    Móricz, Ágnes M; Ott, Péter G; Yüce, Imanuel; Darcsi, András; Béni, Szabolcs; Morlock, Gertrud E

    2018-01-19

    High-performance thin-layer chromatography (HPTLC) coupled with effect-directed analysis was used for non-targeted screening of sunflower leaf extract for components exhibiting antioxidant, antibacterial and/or cholinesterase enzyme inhibitory effects. The active compounds were characterized by HPTLC-electrospray ionization-high resolution mass spectrometry (ESI-HRMS) and HPTLC-Direct Analysis in Real Time (DART)-MS/MS. The latter ambient ionization technique (less soft than ESI) resulted in oxidation and fragmentation products and characteristic fragment ions. NMR spectroscopy after targeted isolation via preparative normal phase flash chromatography and semi-preparative reversed phase high-performance liquid chromatography supported the identification of two diterpenes to be (-)-kaur-16-en-19-oic acid and 15-α-angeloyloxy-ent-kaur-16-en-19-oic acid. Both compounds found to be multi-potent as they inhibited acetylcholinesterase and butyrylcholinesterase and showed antibacterial effects against Gram-positive Bacillus subtilis and Gram-negative Aliivibrio fischeri bacteria. Kaurenoic acid was also active against the Gram-negative pepper pathogenic Xanthomonas euvesicatoria bacteria. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. COMBINED INFORMATION FROM RETARDATION FACTOR (RF) VALUES AND COLOR-REACTIONS ON THE PLATE GREATLY ENHANCES THE IDENTIFICATION POWER OF THIN-LAYER CHROMATOGRAPHY IN SYSTEMATIC TOXICOLOGICAL ANALYSIS

    NARCIS (Netherlands)

    HEGGE, HFJ; FRANKE, JP; DEZEEUW, RA

    A numerical color coding system has been developed to describe the colors of spots obtained after using location reagents in thin-layer chromatography (TLC). This system makes color reactions on the plate amenable to computer handling, so that the retardation factor (Rf) values plus color reactions

  1. Separation of the Carotenoid Bixin from Annatto Seeds Using Thin-Layer and Column Chromatography

    Science.gov (United States)

    McCullagh, James V.; Ramos, Nicholas

    2008-01-01

    In this experiment the carotenoid bixin is isolated from annatto ("Bixa orellana") seeds using column chromatography. The experiment has several key advantages over previous pigment separation experiments. First, unlike other experiments significant quantities of the carotenoid (typically 20 to 25 mg) can be isolated from small quantities of plant…

  2. Assessment of aflatoxin B1 in livestock feed and feed ingredients by high-performance thin layer chromatography

    Directory of Open Access Journals (Sweden)

    Korrapati Kotinagu

    2015-12-01

    Full Text Available Aim: Detection of aflatoxin B1 in Livestock compound Feed and feed ingredients by high-performance thin layer chromatography (HPTLC. Materials and Methods: Chromatography was performed on HPTLC silica gel 60 F 254, aluminum sheets by CAMAG automatic TLC sampler 4, with mobile phase condition chloroform:acetone:water (28:4:0.06. Extraction of aflatoxin B1 from samples was done as per AOAC method and screening and quantification done by HPTLC Scanner 4 under wavelength 366 nm. Results: A total of 97 livestock feed (48 and feed ingredients (49 samples received from different livestock farms and farmers were analyzed for aflatoxin B1of which 29 samples were contaminated, constituting 30%. Out of 48 livestock compound feed samples, aflatoxin B1 could be detected in 16 samples representing 33%, whereas in livestock feed ingredients out of 49 samples, 13 found positive for aflatoxin B1 representing 24.5%. Conclusion: HPTLC assures good recovery, precision, and linearity in the quantitative determination of aflatoxin B1 extracted from Livestock compound feed and feed ingredients. As more number of feed and feed ingredients are contaminated with aflatoxin B1 which causes deleterious effects in both animal and human beings, so there is a need for identifying the source of contamination, executing control measures, enabling better risk assessment techniques, and providing economic benefits.

  3. Semiquantitative determination of polychlorinated biphenyls in tissue samples by thin layer chromatography

    Science.gov (United States)

    Mulhern, B.M.; Cromartie, E.; Reichel, W.L.; Belisle, A.A.

    1971-01-01

    A method is described for the analysis of polychlorinated biphenyl (PCB) compounds in tissue samples. Cleanup by hexane-aceto-nitrile partitioning and Florisil column chromatography are performed on samples before oxidative treatment to convert DDE to DCBP. PCB components are then determined semi-quantitatively by TLC. No prior separation of PCB from chlorinated pesticides is required. The lower limit of sensitivity is 0.2 ?g.

  4. Combined urea-thin layer chromatography and silver nitrate-thin layer chromatography for micro separation and determination of hard-to-detect branched chain fatty acids in natural lipids.

    Science.gov (United States)

    Yan, Yuanyuan; Wang, Xingguo; Liu, Yijun; Xiang, Jingying; Wang, Xiaosan; Zhang, Huijun; Yao, Yunping; Liu, Ruijie; Zou, Xiaoqiang; Huang, Jianhua; Jin, Qingzhe

    2015-12-18

    A simple, fast and efficient procedure was developed for micro separation and enrichment of branched chain fatty acids (BCFA) from natural products using successive thin layer chromatography (TLC) technique coupling novel urea-TLC with AgNO3-TLC, which rely on the formation of urea adduction and AgNO3 bonding in methanol. These natural lipids contain a significant amount of straight chain fatty acids (FA). Fresh and fast urea-TLC and AgNO3-TLC plate making techniques were developed with more even coating and less coating material contamination before being utilized for separation. Goat milk fat was used as a model. Various experimental parameters that affect urea-TLC and AgNO3-TLC separation of BCFA were investigated and optimized, including coating of urea, concentration of original oil sample, mobile phase and sample application format. High efficiency of removal of straight chain FA was achieved with a low amount of sample in an easy and fast way. A total BCFA mix with much higher purity than previous studies was successfully achieved. The developed method has also been applied for the concentration and analysis of BCFA in cow milk fat and Anchovy oil. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Combined thin layer chromatography and gas chromatography with mass spectrometric analysis of lipid classes and fatty acids in malnourished polar bears (Ursus maritimus) which swam to Iceland.

    Science.gov (United States)

    Eibler, Dorothee; Krüger, Sabine; Skírnisson, Karl; Vetter, Walter

    2017-03-01

    Between 2008 and 2011, four polar bears (Ursus maritimus) from the Greenland population swam and/or drifted on ice to Iceland where they arrived in very poor body condition. Body fat resources in these animals were only between 0% and 10% of the body weight (usually 25%). Here we studied the lipid composition in different tissues (adipose tissue if available, liver, kidney and muscle). Lipid classes were determined by thin layer chromatography (TLC) and on-column gas chromatography with mass spectrometry (GC/MS). The fatty acid pattern of total lipids and free fatty acids was analyzed by GC/MS in selected ion monitoring (SIM) mode. Additionally, cholesteryl esters and native fatty acid methyl esters, initially detected as zones in thin layer chromatograms, were enriched by solid phase extraction and quantified by GC/MS. The ratio of free fatty acids to native fatty acid methyl esters could be correlated with the remained body lipids in the polar bears and thus may also serve as a marker for other starving animals or even for humans. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Analysis of biodiesel conversion using thin layer chromatography and nonlinear calibration curves

    DEFF Research Database (Denmark)

    Fedosov, Sergey; Brask, Jesper; Xu, Xuebing

    2011-01-01

    chromatography (TLC) for this purpose, where the detection was based on either flame ionization detector (FID) or a modified staining procedure. The suggested staining method gave no background and appeared well suited for quantitative analysis. The relevant calibrations are presented, and the general principles...... were separated and quantified. Relation of the BD contents measured by TLC and GC gave the values of 1.03 ± 0.07 (TLC-staining) and 0.95 ± 0.04 (TLC–FID), indicating applicability of the TLC-methods....

  7. Thin-layer chromatography and mass spectrometry coupled using proximal probe thermal desorption with electrospray or atmospheric pressure chemica lionization

    Energy Technology Data Exchange (ETDEWEB)

    Ovchinnikova, Olga S [ORNL; Van Berkel, Gary J [ORNL

    2010-01-01

    An atmospheric pressure proximal probe thermal desorption sampling method coupled with secondary ionization by electrospray or atmospheric pressure chemical ionization was demonstrated for the mass spectrometric analysis of a diverse set of compounds (dyestuffs, pharmaceuticals, explosives and pesticides) separated on various high-performance thin-layer chromatography plates. Line scans along or through development lanes on the plates were carried out by moving the plate relative to a stationary heated probe positioned close to or just touching the stationary phase surface. Vapors of the compounds thermally desorbed from the surface were drawn into the ionization region of a combined electrospray ionization/atmospheric pressure chemical ionization source where they merged with reagent ions and/or charged droplets from a corona discharge or an electrospray emitter and were ionized. The ionized components were then drawn through the atmospheric pressure sampling orifice into the vacuum region of a triple quadrupole mass spectrometer and detected using full scan, single ion monitoring, or selected reaction monitoring mode. Studies of variable parameters and performance metrics including the proximal probe temperature, gas flow rate into the ionization region, surface scan speed, read-out resolution, detection limits, and surface type are discussed.

  8. Evaluation of group of Alpinia galanga n-hexane-Extract against Candida albicans by bioautography and thin layer chromatography

    Directory of Open Access Journals (Sweden)

    Eni Kusumaningtyas

    2008-12-01

    Full Text Available Alpinia galanga has been used for centuries as a remedy for human diseases because it contains of therapeutic compounds. The objectives of this study was to define groups of the antifungal compounds of Alpinia galangal n-hexane-extract. Alpinia galanga was extracted by maceration method and the compounds were analyzed by phytochemical analysis. The extract was run on the thin layer chromatography (TLC plate silica gel GF254 with dichloromethane and toluene. Bioautography was conducted to determine antifungal compounds against Candida albicans. Active compounds on the previous step were identified by running extract on TLC plate and sprayed with Vanilin sulphuric acid and Liebermann-Burchard I. The results of phytochemical analysis showed that Alpinia galanga n-hexane-extract contains alkaloids, flavonoids, saponins, triterpenoid, tannins and aromatic oil. Bioautogram revealed that there was one inhibition zone against Candida albicans. The active compounds in the inhibition zone were in Rf value 0.75 and 0.89. One out of the two compounds was identified as a compound from terpenoid group.

  9. Tuneable surface enhanced Raman spectroscopy hyphenated to chemically derivatized thin-layer chromatography plates for screening histamine in fish.

    Science.gov (United States)

    Xie, Zhengjun; Wang, Yang; Chen, Yisheng; Xu, Xueming; Jin, Zhengyu; Ding, Yunlian; Yang, Na; Wu, Fengfeng

    2017-09-01

    Reliable screening of histamine in fish was of urgent importance for food safety. This work presented a highly selective surface enhanced Raman spectroscopy (SERS) method mediated by thin-layer chromatography (TLC), which was tailored for identification and quantitation of histamine. Following separation and derivatization with fluram, plates were assayed with SERS, jointly using silver nanoparticle and NaCl. The latter dramatically suppressed the masking effect caused by excessive fluram throughout the plate, thus offering clear baseline and intensive Raman fingerprints specific to the analyte. Under optimized conditions, the usability of this method was validated by identifying the structural fingerprints of both targeted and unknown compounds in fish samples. Meanwhile, the quantitative results of this method agreed with those by an HPLC method officially suggested by EU for histamine determination. Showing remarkable cost-efficiency and user-friendliness, this facile TLC-SERS method was indeed screening-oriented and may be more attractive to controlling laboratories of limited resource. Copyright © 2017 Elsevier Ltd. All rights reserved.

  10. Changes in fluorescent emission due to non-covalent interactions as a general detection procedure for thin-layer chromatography.

    Science.gov (United States)

    Cebolla, Vicente L; Mateos, Elena; Garriga, Rosa; Jarne, Carmen; Membrado, Luis; Cossío, Fernando P; Gálvez, Eva M; Matt, Muriel; Delgado-Camón, Arantzazu

    2012-01-16

    Changes in fluorescence emission due to non-covalent analyte-fluorophore interactions in silica gel plates are studied and used as a general detection procedure for thin-layer chromatography (TLC). The presence of the analyte modifies the microenvironment of the fluorophore and thus changes the balance between radiative (k(r)) and non-radiative (k(nr)) emission constants. A model is proposed for analyte-fluorophore induced electrostatic interactions, which depend on analyte polarizability and are responsible for fluorescence enhancements. As consequence of these induced interactions, the analyte creates an apolar environment that prevents non-fluorescent decay mechanisms, decreasing k(nr). On the other hand, the effect of an increase in refractive index on k(r) is investigated, as it contributes to some extent to fluorescence enhancements in silica gel medium. Changes in fluorescence emission should be regarded as a general property of fluorophores in the presence of analytes, and criteria that fluorophores should meet to be used as sensitive TLC probes are discussed here. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. An improved thin-layer chromatography/mass spectrometry coupling using a surface sampling probe electrospray ion trap system

    Energy Technology Data Exchange (ETDEWEB)

    Ford, Michael J [ORNL; Van Berkel, Gary J [ORNL

    2004-01-01

    A combined surface sampling probe/electrospray emitter coupled with an ion trap mass spectrometer was used for the direct read out of unmodified reversed-phase C18 thin-layer chromatography (TLC) plates. The operation of the surface sampling electrospray ionization interface in positive and negative ionization modes was demonstrated through the direct analysis of TLC plates on which a commercial test mix comprised of four dye compounds viz., rhodamine B, fluorescein, naphthol blue black, and fast green FCF, and an extract of the caffeine-containing plant Ilex vomitoria, were spotted and developed. Acquisition of full-scan mass spectra and automated collection of MS/MS product ion spectra while scanning a development lane along the surface of a TLC plate demonstrated the advantages of using an ion trap in this combination. Details of the sampling system, benefits of analyzing a developed lane in both positive ion and negative ion modes, levels of detection while surface scanning, surface scan speed effects, and the utility of three-dimensional data display, are also discussed.

  12. Detection of adulterated copaiba (Copaifera multijuga Hayne oil-resins by refractive index and thin layer chromatography

    Directory of Open Access Journals (Sweden)

    Karol de S. Barbosa

    Full Text Available The refractive indices (RI of the eight samples of copaiba oils, collected for this study at RDS Tupé ranged from 1.50284 to 1.50786. The thin layer chromatography (TLC plates of these oils revealed with anisaldehyde-sulphuric acid reagent showed dark lilac stains with several small stains at low Rf and a large rounded stain at high Rf. On the other hand, the twelve copaiba oils purchased at local markets presented RI between 1.48176 and 1.50886, and the TLC plates, showed as general profile blue stains, with smaller superimposed stains at low Rf, bigger superimposed stains like elongated stain at high Rf and a colorless rounded stain at middle Rf. Among 12 purchased oils at local markets, a three oil-resins presented similar RI and TLC profile to those observed for collected copaiba oils; b six oils showed same RI and TLC profiles to those observed for soybean oil; c three samples presented RI near to those showed by copaiba oil-resin, however the TLC profile was near to profile observed for a prepared mixture soybean oil: copaiba oil, two samples with 3:1 proportion and one sample with 1:3 proportion. Therefore, the RI determination and the TLC profiles could be considered rapid and efficient procedures for detection of vegetal oil in the copaiba oil-resins.

  13. Joint IDF-IUPAC-IAEA(FAO) interlaboratory validation for determining aflatoxin M1 in milk by using immunoaffinity clean-up before thin-layer chromatography.

    Science.gov (United States)

    Grosso, F; Fremy, J M; Bevis, S; Dragacci, S

    2004-04-01

    A collaborative study was conducted under the auspices of the International Dairy Federation (IDF), the International Union of Pure and Applied Chemistry (IUPAC) and the International Atomic Energy Agency (IAEA), a collaborative Food and Agricultural Organization (FAO) body fully to validate a method combining immunoaffinity clean-up to thin-layer chromatography for the determination of aflatoxin M(1) in milk. Work was done in order to afford those laboratories not equipped with high-performance liquid chromatography, mainly from developing countries, with a simplified but fully validated method as an alternative to the European validated immunoaffinity-high performance liquid chromatography method published as an EN ISO Standard 14501, February 1999. The validation study was carried out on samples of aflatoxin M(1)-contaminated milk and milk powder at levels close to the tolerable level of 0.5 microg l(-1) as recommended by the Codex Alimentarius and to the regulatory level of 0.05 microg l(-1) as laid down by the European Commission. Fourteen laboratories representing 11 countries participated in the trial. The relative standard deviations for repeatability and reproducibility based on raw data were in the range 27-48 and 35-54%, respectively. The recovery rate varied from 32 to 120%. The mishandling of two crucial steps of the protocol such as matrix sample reconstitution and extract evaporation could explain the wide variation of the recovery rate. For this reason, data were then corrected for recovery. Consequently, the relative standard deviations for repeatability and reproducibility were recalculated after correction for recovery and were in the range 26-54 and 34-53%, respectively. The method will be published as a standard ISO/DIS 14674--IDF 190.

  14. Determination of 6-gingerol in ginger (Zingiber officinale) using high-performance thin-layer chromatography.

    Science.gov (United States)

    Rai, Sujay; Mukherjee, Kakali; Mal, Mainak; Wahile, Atul; Saha, Bishnu Pada; Mukherjee, Pulok K

    2006-10-01

    A sensitive and accurate High-Performance TLC (HPTLC) method has been developed to determine the quantity of 6-gingerol in rhizomes of Zingiber officinale (family: Zingiberaceae), commonly known as ginger. Methanol extracts of rhizomes from three different sources were used for HPTLC, n-hexane, and diethyl ether (40:60 v/v) as the mobile phase. The Rf of 6-gingerol was found to be 0.40. The calibration plot was linear in the range of 250-1200 ng of 6-gingerol and the correlation coefficient of 0.9997 was indicative of good linear dependence of peak area on concentration. The mean quantity of 6-gingerol was found to be 60.44+/-2.53 mg/g of ginger extract. The method permits reliable quantification of 6-gingerol and good resolution and separation of 6-gingerol from other constituents of ginger. To study the accuracy and precision of the method, recovery studies were performed by the method of standard addition. Recovery values from 99.79 to 99.84% showed the excellent reliability and reproducibility of the method. The proposed HPTLC method for quantitative monitoring of 6-gingerol in ginger can be used for routine quality testing of ginger extracts.

  15. Phosphorolytic activity of Escherichia coli glycyl-tRNA synthetase towards its cognate aminoacyl adenylate detected by 31P-NMR spectroscopy and thin-layer chromatography

    DEFF Research Database (Denmark)

    Led, Jens Jørgen; Switon, Werner K.; Jensen, Kaj Frank

    1983-01-01

    The catalytic activity of highly purified Escherichia coli glycyl-tRNA synthetase has been studied by 31P-NMR spectroscopy and thin-layer chromatography on poly(ethyleneimine)-cellulose. It was found that this synthetase, besides the activation of its cognate amino acid and the syntheses of adeno......The catalytic activity of highly purified Escherichia coli glycyl-tRNA synthetase has been studied by 31P-NMR spectroscopy and thin-layer chromatography on poly(ethyleneimine)-cellulose. It was found that this synthetase, besides the activation of its cognate amino acid and the syntheses...... catalytic activities of aminoacyl-tRNA synthetases is discussed, as well as the biological significance of the reaction....

  16. Evaluation of thin-layer chromatography methods for quality control of commercial products containing Aesculus hippocastanum, Turnera diffusa, Matricaria recutita, Passiflora incarnata, and Tilia occidentalis.

    Science.gov (United States)

    Ramírez-Durón, Rosalba; Ceniceros-Almaguer, Lucía; Salazar-Aranda, Ricardo; Salazar-Cavazos, Ma de la Luz; Waksman de Torres, Noemi

    2007-01-01

    In Mexico, plant-derived products with health claims are sold as herbal dietary supplements, and there are no rules for their legal quality control. Aesculus hippocastanum, Turnera diffusa, Matricaria recutita, Passiflora incarnata, and Tilia occidentalis are some of the major commercial products obtained from plants used in this region. In this paper, we describe the effectiveness of thin-layer chromatography methods to provide for the quality control of several commercial products containing these plants. Standardized extracts were used. Of the 49 commercial products analyzed, only 32.65% matched the chromatographic characteristic of standardized extracts. A significant number of commercial products did not match their label, indicating a problem resulting from the lack of regulation for these products. The proposed methods are simple, sensitive, and specific and can be used for routine quality control of raw herbals and formulations of the tested plants. The results obtained show the need to develop simple and reliable analytical methods that can be performed in any laboratory for the purpose of quality control of dietary supplements or commercial herbal products sold in Mexico.

  17. Simultaneous Analysis of Losartan Potassium, Amlodipine Besylate, and Hydrochlorothiazide in Bulk and in Tablets by High-Performance Thin Layer Chromatography with UV-Absorption Densitometry

    Directory of Open Access Journals (Sweden)

    Karunanidhi Santhana Lakshmi

    2012-01-01

    Full Text Available A Simple high-performance thin layer chromatography (HPTLC method for separation and quantitative analysis of losartan potassium, amlodipine, and hydrochlorothiazide in bulk and in pharmaceutical formulations has been established and validated. After extraction with methanol, sample and standard solutions were applied to silica gel plates and developed with chloroform : methanol : acetone : formic acid 7.5 : 1.3 : 0.5 : 0.03 (/// as mobile phase. Zones were scanned densitometrically at 254 nm. The values of amlodipine besylate, hydrochlorothiazide, and losartan potassium were 0.35, 0.57, and 0.74, respectively. Calibration plots were linear in the ranges 500–3000 ng per spot for losartan potassium, amlodipine and hydrochlorothiazide, the correlation coefficients, r, were 0.998, 0.998, and 0.999, respectively. The suitability of this method for quantitative determination of these compounds was by validation in accordance with the requirements of pharmaceutical regulatory standards. The method can be used for routine analysis of these drugs in bulk and in formulation.

  18. Thin layer chromatography fingerprint, antioxidant, and antibacterial activities of rhizomes, stems, and leaves of Curcuma aeruginosa Roxb.

    Science.gov (United States)

    Safitri, A.; Batubara, I.; Khumaida, N.

    2017-05-01

    Fingerprints of 5 temu hitam (Curcuma aeruginosa Roxb.) accessions (Malang, Cirebon, Kuningan 1, Bogor, and Liwa) were determined by thin-layer chromatography (TLC) and compared to fingerprints of turmeric (Curcuma longa L), temu putih (Curcuma zedoaria (Christm.) Roscoe), and temu lawak (Curcuma zanthorriza Roxb.). Maceration method with ethanol as the solvent was used for extraction. The eluent used for fingerprint by TLC was chloroform:dichloromethane (9:1v/v). Five accessions of temu hitam show similar fingerprint patterns, but different in band thickness. Temu hitam rhizomes have bands of curcuminoid (Rf 0.22, 0.10, 0.03), and characteristic bands of Rf 0.42, 0.27, and 0.77, which can be distinguished from turmeric and temu lawak and Rf 0.13, which is different from temu putih. Leaves and stems of temu hitam can be distinguished from temu putih, turmeric, and temu lawak at Rf 0.60. Rhizomes of all plants reveal strong antibacterial activity against Staphylococcus aureus and antioxidant activity on DPPH radicals than its corresponding stems and leaves. Antibacterial and antioxidant activities were determined by microdilution and TLC-bioautography. Antibacterial activity of rhizomes of Cirebon and Kuningan 1 accessions are higher than that of other accessions (MIC = 250 μg/mL MBC = 500 μg/mL, but lower as compared to that of temu lawak (MIC = 62.5 μg/mL, MBC = 250 μg/mL) and tetracycline (MIC = MBC = 15.63 μg/mL). Rhizome of Liwa accession exhibits the highest antioxidant activity (IC50 = 124.88 μg/mL) amongst all accessions, but lower than that of temu lawak (IC50 = 18.45 μg/mL), turmeric (IC50 = 18.82 μg/mL), and temu putih (IC50 = 94.35 μg/mL).

  19. Rapid identification of siderophores by combined thin-layer chromatography/matrix-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Hayen, Heiko; Volmer, Dietrich A

    2005-01-01

    The investigation of a combined thin-layer chromatography/matrix-assisted laser desorption/ionization mass spectrometry (TLC/MALDI-MS) method for the analysis of siderophores from microbial samples is described. The investigated siderophores were enterobactin, ferrioxamine B, ferrichrome, ferrirhodin, rhodotorulic acid and coprogen. Solid-phase extraction was employed to recover the siderophores from the microbial samples. After visualization of the spots via spraying with ferric chloride or chrome azurol sulfonate assay solution, the MALDI matrix was applied to the gel surface. Several TLC/MALDI experimental parameters were optimized, such as type and concentration of MALDI matrix, as well as the type and composition of solvent to facilitate analyte transport from the inside of the TLC gel to the surface. The impact of these parameters on sensitivity, precision and ion formation of the various siderophores was studied. The detection limits for the investigated siderophores were in the range 1-4 pmol. These values were about 4-24 times higher than the detection limits obtained directly from stainless steel MALDI targets. The differences were most likely due to incomplete transport of the 'trapped' analyte molecules from the deeper layers of the TLC gel to the surface and into the matrix layer. In addition, chromatographic band broadening spread the analyte further in TLC as compared with the steel plates, resulting in less analyte per surface area. The identification of the siderophores was aided by concurrently applying a Ga(III) nitrate solution to the TLC plate during the visualization step. The resulting formation of Ga(III) complexes lead to distinctive (69)Ga/(71)Ga isotope patterns in the mass spectra. The versatility of the TLC/MALDI-MS assay was demonstrated by using it to analyze siderophores in a Pseudomonas aeruginosa sample. An iron-binding compound was identified in the sample, namely pyochelin (2-(2-o-hydroxyphenyl-2-thiazolin-4-yl)-3

  20. Determination of caffeine, theobromine and theophylline in Mate beer and Mate soft drinks by high-performance thin-layer chromatography.

    Science.gov (United States)

    Oellig, Claudia; Schunck, Jacob; Schwack, Wolfgang

    2018-01-19

    Mate beer and Mate soft drinks are beverages produced from the dried leaves of Ilex paraguariensis (Yerba Mate). In Yerba Mate, the xanthine derivatives caffeine, theobromine and theophylline, also known as methylxanthines, are important active components. The presented method for the determination of caffeine, theobromine and theophylline in Mate beer and Mate soft drinks by high-performance thin-layer chromatography with ultraviolet detection (HPTLC-UV) offers a fully automated and sensitive determination of the three methylxanthines. Filtration of the samples was followed by degassing, dilution with acetonitrile in the case of Mate beers for protein precipitation, and centrifugation before the extracts were analyzed by HPTLC-UV on LiChrospher silica gel plates with fluorescence indicator and acetone/toluene/chloroform (4:3:3, v/v/v) as the mobile phase. For quantitation, the absorbance was scanned at 274nm. Limits of detection and quantitation were 1 and 4ng/zone, respectively, for caffeine, theobromine and theophylline. With recoveries close to 100% and low standard deviations reliable results were guaranteed. Experimental Mate beers as well as Mate beers and Mate soft drinks from the market were analyzed for their concentrations of methylxanthines. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. Screening for 16-O-methylcafestol in roasted coffee by high-performance thin-layer chromatography-fluorescence detection - Determination of Coffea canephora admixtures to Coffea arabica.

    Science.gov (United States)

    Oellig, Claudia; Radovanovic, Jessica

    2017-10-12

    16-O-Methylcafestol (16-OMC), the characteristic diterpene exclusively present in Coffea canephora, is an excellent marker for Coffea canephora admixtures to Coffea arabica. Here we show a straightforward, selective and sensitive screening method for the determination of 16-OMC in roasted coffee by high-performance thin-layer chromatography with fluorescence detection (HPTLC-FLD). As internal standard, Sudan IV was used, and a direct saponification with 10% ethanolic potassium hydroxide solution was followed by solid supported liquid extraction with petroleum ether. 16-OMC was selectively derivatized with 2-naphthoyl chloride and analyzed by HPTLC-FLD on silica gel plates with cyclohexane/tert-butyl methyl ether/formic acid (86:14:2, v/v/v) as the mobile phase. The enhanced fluorescence was scanned at UV 244/>320nm. Limits of detection and quantitation of 5 and 14mg 16-OMC/kg coffee allowed the determination of Coffea canephora admixtures to Coffea arabica below 1%. Recoveries for blends of Coffea arabica with Coffea canephora were close to 100%. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Stability-indicating assay of repaglinide in bulk and optimized nanoemulsion by validated high performance thin layer chromatography technique

    Directory of Open Access Journals (Sweden)

    Juber Akhtar

    2013-01-01

    Full Text Available A sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC method for analysis of repaglinide both as a bulk drug and in nanoemulsion formulation was developed and validated. The method employed TLC aluminum plates precoated with silica gel 60F-254 as the stationary phase. The solvent system consisted of chloroform/methanol/ammonia/glacial acetic acid (7.5:1.5:0.9:0.1, v/v/v/v. This system was found to give compact spots for repaglinide (R f value of 0.38 ± 0.02. Repaglinide was subjected to acid and alkali hydrolysis, oxidation, photodegradation and dry heat treatment. Also, the degraded products were well separated from the pure drug. Densitometric analysis of repaglinide was carried out in the absorbance mode at 240 nm. The linear regression data for the calibration plots showed good linear relationship with r 2 = 0.998 ± 0.032 in the concentration range of 50-800 ng. The method was validated for precision, accuracy as recovery, robustness and specificity. The limits of detection and quantitation were 0.023 and 0.069 ng per spot, respectively. The drug undergoes degradation under acidic and basic conditions, oxidation and dry heat treatment. All the peaks of the degraded product were resolved from the standard drug with significantly different R f values. Statistical analysis proves that the method is reproducible and selective for the estimation of the said drug. As the method could effectively separate the drug from its degradation products, it can be employed as a stability-indicating one. Moreover, the proposed HPTLC method was utilized to investigate the degradation kinetics in 1M NaOH.

  3. Assessment of antioxidant activity in Victorian marine algal extracts using high performance thin-layer chromatography and multivariate analysis.

    Science.gov (United States)

    Agatonovic-Kustrin, Snezana; Morton, David W; Ristivojević, Petar

    2016-10-14

    The aim of this study was to develop and validate a rapid and simple high performance thin layer chromatographic (HPTLC) method to screen for antioxidant activity in algal samples. 16 algal species were collected from local Victorian beaches. Fucoxanthin, one of the most abundant marine carotenoids was quantified directly from the HPTLC plates before derivatization, while derivatization either with 2,2-diphenyl-1-picrylhydrazyl (DPPH) or ferric chloride (FeCl 3 ) was used to analyze antioxidants in marine algae, based on their ability to scavenge non biological stable free radical (DPPH) or to chelate iron ions. Principal component analysis of obtained HPTLC fingerprints has classified algae species into 5 groups according to their chemical/antioxidant profiles. The investigated brown algae samples were found to be rich in non-and moderate-polar compounds and phenolic compounds with antioxidant activity. Most of the phenolic iron chelators also have shown free radical scavenging activity. Strong positive and significant correlations between total phenolic content and DPPH radical scavenging activity showed that, phenolic compounds, including flavonoids are the main contributors of antioxidant activity in these species. The results suggest that certain brown algae possess significantly higher antioxidant potential when compared to red or green algae and could be considered for future applications in medicine, dietary supplements, cosmetics or food industries. Cystophora monilifera extract was found to have the highest antioxidant concentration, followed by Zonaria angustata, Cystophora pectinate, Codium fragile, and Cystophora pectinata. Fucoxanthin was found mainly in the brown algae species. The proposed methods provide an edge in terms of screening for antioxidants and quantification of antioxidant constituents in complex mixtures. The current application also demonstrates flexibility and versatility of a standard HPTLC system in the drug discovery. Proposed

  4. Thin-layer chromatography immunostaining in detecting anti-phospholipid antibodies in seronegative anti-phospholipid syndrome.

    Science.gov (United States)

    Conti, F; Alessandri, C; Sorice, M; Capozzi, A; Longo, A; Garofalo, T; Misasi, R; Bompane, D; Hughes, G R V; Khamashta, M A; Valesini, G

    2012-03-01

    In clinical practice it is possible to find patients with clinical signs suggestive of anti-phospholipid syndrome (APS) who are persistently negative for the routinely used anti-phospholipid antibodies (aPL). Therefore, the term proposed for these cases was seronegative APS (SN-APS). We investigated the clinical usefulness of thin-layer chromatography (TLC) immunostaining in detecting serum aPL in patients presenting clinical features of SN-APS. Sera from 36 patients with SN-APS, 19 patients with APS, 18 patients with systemic lupus erythematosus (SLE), 20 anti-hepatitis C virus (HCV)-positive subjects and 32 healthy controls were examined for aPL using TLC immunostaining. Anti-β(2) -glycoprotein-I, anti-annexin II, anti-annexin V and anti-prothrombin antibodies were tested by enzyme-linked immunosorbent assays (ELISA). Eahy926, a human-derived endothelial cell line, was incubated with immunoglobulin (Ig)G fraction from SN-APS patients and analysis of phospho-interleukin (IL)-1 receptor-associated kinase (IRAK) and phospho-nuclear factor (NF)-κB was performed by Western blot, vascular cell adhesion molecule 1 (VCAM-1) expression by cytofluorimetric analysis and supernatants tissue factor (TF) levels by ELISA. TLC immunostaining showed aPL in 58·3% of SN-APS patients: anti-cardiolipin in 47·2%, anti-lyso(bis)phosphatidic acid in 41·7% and anti-phosphatidylethanolamine in 30·5%. Six of 36 patients showed anti-annexin II. Incubation of Eahy926 cells with IgG from SN-APS induced IRAK phosphorylation, NF-κB activation, VCAM-1 surface expression and TF cell release. TLC immunostaining could identify the presence of aPL in patients with SN-APS. Moreover, the results suggest the proinflammatory and procoagulant effects in vitro of these antibodies. © 2011 The Authors. Clinical and Experimental Immunology © 2011 British Society for Immunology.

  5. An Improved Method for the Extraction and Thin-Layer Chromatography of Chlorophyll A and B from Spinach

    Science.gov (United States)

    Quach, Hao T.; Steeper, Robert L.; Griffin, William G.

    2004-01-01

    A simple and fast method, which resolves chlorophyll a and b from spinach leaves on analytical plates while minimizing the appearance of chlorophyll degradation products is shown. An improved mobile phase for the Thin-layer chromatographic analysis of spinach extract that allows for the complete resolution of the common plant pigments found in…

  6. Investigation of Symphytum cordatum alkaloids by liquid-liquid partitioning, thin-layer chromatography and liquid chromatography-ion-trap mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mroczek, Tomasz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland)]. E-mail: tmroczek@pharmacognosy.org; Ndjoko-Ioset, Karine [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland); Glowniak, Kazimierz [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Mietkiewicz-Capala, Agnieszka [Department of Pharmacognosy with Medicinal Plants Laboratory, Medical University, 1 Chodzki St., 20-093 Lublin (Poland); Hostettmann, Kurt [Laboratoire de Pharmacognosie et Phytochimie, Ecole de Pharmacie Geneve-Lausanne, Universite de Geneve, Quai Ernest-Ansermet 30, CH-1211 Geneva 4 (Switzerland)

    2006-05-04

    From the alkalised crude extract of Symphytum cordatum (L.) W.K. roots, pyrrolizidine alkaloids (PAs) were extracted as free tertiary bases and polar N-oxides in a merely one-step liquid-liquid partitioning (LLP) in separation funnel and subsequently pre-fractionated by preparative multiple-development (MD) thin-layer chromatography (TLC) on silica gel plates. In this way three alkaloid fractions of different polarities and retention on silica gel plates were obtained as: the most polar N-oxides of the highest retention, the tertiary bases of medium retention, and diesterified N-oxides of the lowest retention. The former fraction was reduced into free bases by sodium hydrosulfite and purified by LLP on Extrelut-NT3 cartridge. It was further analysed together with the two other fractions by high-performance liquid chromatography (HPLC)-ion-trap mass spectrometry with atmospheric pressure chemical ionization (APCI) interface on XTerra C{sub 18} column using a gradient elution. Based on MS {sup n} spectra, 18 various alkaloids have been tentatively determined for the first time in this plant as the following types of structure: echimidine-N-oxide (three diasteroisomers), 7-sarracinyl-9-viridiflorylretronecine (two diasteroisomers), echimidine (two diasteroisomers), lycopsamine (two diasteroisomers), dihydroechinatine-N-oxide, dihydroheliospathuline-N-oxide, lycopsamine-N-oxide (three diasteroisomers), 7-acetyllycopsamine-N-oxide, symphytine-N-oxide (two diasteroisomers) and 2'',3''-epoxyechiumine-N-oxide.

  7. Lipophilic properties of anti-Alzheimer's agents determined by micellar electrokinetic chromatography and reversed-phase thin-layer chromatography.

    Science.gov (United States)

    Godyń, Justyna; Hebda, Michalina; Więckowska, Anna; Więckowski, Krzysztof; Malawska, Barbara; Bajda, Marek

    2017-05-01

    Lipophilicity as one of the most important physicochemical properties of the biologically active compounds is closely related to their pharmacokinetic parameters and therefore, it is taken into account at the design stage of new drugs. Among the novel, fast, and reliable methods for determination of the lipophilicity of compounds micellar electrokinetic chromatography (MEKC) is considered to be an appropriate one for bioactive molecules, as it closely mimics the physiological conditions. In this paper MEKC was used for the estimation of log P values for 49 derivatives of phthalimide, tetrahydroisochinoline and indole, designed and synthesized as potential anti-Alzheimer's agents with cholinesterase inhibitory activity. RP-TLC method was applied for determination of another lipophilicity descriptor - RM0 . The results of both experimental methods were compared with each other giving satisfactory correlation (R = 0.784), and with computational methods (Marvin, ChemOffice Software) resulting in weaker correlation (R = 0.466-0.687). The lipophilicity-activity relationship was finally established, showing significant influence of lipophilicity on cholinesterase inhibition in some subgroups of phthalimide derivatives. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Óleo essencial de limão no ensino da cromatografia em camada delgada Lime essential oil in the teaching of thin layer chromatography

    Directory of Open Access Journals (Sweden)

    Rosaly S. Silva

    2009-01-01

    Full Text Available This paper describes a simple experiment employing the essential oil of limes which can be applied in undergraduate organic chemistry laboratory classes for the teaching of thin layer chromatography (TLC. The experiment consists in submit lime peel oil to TLC separation employing hexane and dichloromethane as the eluents and five different systems for visualization of the chromatogram. In one experiment it is possible to teach the different variables of the TLC technique. This experiment may also be performed following vapor distillation and liquid-liquid extraction technique in experimental classes.

  9. Simplified and rapid method for extraction of ergosterol from natural samples and detection with quantitative and semi-quantitative methods using thin-layer chromatography

    OpenAIRE

    Larsen, Cand.scient Thomas; Ravn, Senior scientist Helle; Axelsen, Senior Scientist Jørgen

    2004-01-01

    A new and simplified method for extraction of ergosterol (ergoste-5,7,22-trien-3-beta-ol) from fungi in soil and litter was developed using pre-soaking extraction and paraffin oil for recovery. Recoveries of ergosterol were in the range of 94 - 100% depending on the solvent to oil ratio. Extraction efficiencies equal to heat-assisted extraction treatments were obtained with pre-soaked extraction. Ergosterol was detected with thin-layer chromatography (TLC) using fluorodensitometry with a quan...

  10. Estimation of guggulsterone E and Z in the Guggul-based commercial formulations using high-performance thin-layer chromatography

    Directory of Open Access Journals (Sweden)

    Pramod Kumar Sairkar

    2017-01-01

    Full Text Available Background: Guggulsterone (GS is a plant steroid and bioactive compound present in gum Guggul of Commiphora wightii. An Indian herbal medicine system “Ayurveda” has a long history of use of gum Guggul and plant extract of C. wightii as medicine for the treatment of various illnesses. Complex nature, low availability, and inconsistency of phytoconstituents make its analysis of difficult tasks. Aims: In this work, six different Guggul-based herbal formulations were examined for estimation of GS and their isomers (E and Z through high-performance thin-layer chromatography technique. Materials and Methods: For that various concentrations of standard E-GS and Z-GS (50 ng–250 ng/spot with samples (20 μg/spot were applied on silica gel coated aluminum plate and developed with the mobile phase of toluene: ethyl acetate: formic acid: methanol (6:2:1:0.5. The scanning was performed at 254 nm wavelength and the absorbance (scan spectrum of E-GS and Z-GS peak was generated at 200 nm–400 nm wavelength range. Results and Conclusions: Rf value and scan spectrum pattern of the samples reveal that they contain either one form of GS (E-GS, Z-GS or both. The quantity of E-GS and Z-GS within the samples was ranged from 0.230 ± 0.0040–0.926 ± 0.0168% to 0.537 ± 0.0026–0.723 ± 0.0177%, respectively.

  11. Direct analysis of Salvia divinorum leaves for salvinorin A by thin layer chromatography and desorption electrospray ionization multi-stage tandem mass spectrometry.

    Science.gov (United States)

    Kennedy, Joseph H; Wiseman, Justin M

    2010-05-15

    Salvia divinorum is widely cultivated in the US, Mexico, Central and South America and Europe and is consumed for its ability to produce hallucinogenic effects similar to those of other scheduled hallucinogenic drugs, such as LSD. Salvinorin A (SA), a kappa opiod receptor agonist and psychoactive constituent, is found primarily in the leaves and to a lesser extent in the stems of the plant. Herein, the analysis of intact S. divinorum leaves for SA and of acetone extracts separated using thin layer chromatography (TLC) is demonstrated using desorption electrospray ionization (DESI) mass spectrometry. The detection of SA using DESI in the positive ion mode is characterized by several ions associated with the compound - [M+H](+), [M+NH(4)](+), [M+Na](+), [2M+NH(4)](+), and [2M+Na](+). Confirmation of the identity of these ions is provided through exact mass measurements using a time-of-flight (ToF) mass spectrometer. The presence of SA in the leaves was confirmed by multi-stage tandem mass spectrometry (MS(n)) of the [M+H](+) ion using a linear ion trap mass spectrometer. Direct analysis of the leaves revealed several species of salvinorin in addition to SA as confirmed by MS(n), including salvinorin B, C, D/E, and divinatorin B. Further, the results from DESI imaging of a TLC separation of a commercial leaf extract and an acetone extract of S. divinorum leaves were in concordance with the TLC/DESI-MS results of an authentic salvinorin A standard. The present study provides an example of both the direct analysis of intact plant materials for screening illicit substances and the coupling of TLC and DESI-MS as a simple method for the examination of natural products. Copyright (c) 2010 John Wiley & Sons, Ltd.

  12. Thin Layer Chromatography-Bioautography and Gas Chromatography-Mass Spectrometry of Antimicrobial Leaf Extracts from Philippine Piper betle L. against Multidrug-Resistant Bacteria

    Directory of Open Access Journals (Sweden)

    Demetrio L. Valle

    2016-01-01

    Full Text Available This study isolated and identified the antimicrobial compounds of Philippine Piper betle L. leaf ethanol extracts by thin layer chromatography- (TLC- bioautography and gas chromatography-mass spectrometry (GC-MS. Initially, TLC separation of the leaf ethanol extracts provided a maximum of eight compounds with Rf values of 0.92, 0.86, 0.76, 0.53, 0.40, 0.25, 0.13, and 0.013, best visualized when inspected under UV 366 nm. Agar-overlay bioautography of the isolated compounds demonstrated two spots with Rf values of 0.86 and 0.13 showing inhibitory activities against two Gram-positive multidrug-resistant (MDR bacteria, namely, methicillin-resistant Staphylococcus aureus and vancomycin-resistant Enterococcus. The compound with an Rf value of 0.86 also possessed inhibitory activity against Gram-negative MDR bacteria, namely, carbapenem-resistant Enterobacteriaceae-Klebsiella pneumoniae and metallo-β-lactamase-producing Acinetobacter baumannii. GC-MS was performed to identify the semivolatile and volatile compounds present in the leaf ethanol extracts. Six compounds were identified, four of which are new compounds that have not been mentioned in the medical literature. The chemical compounds isolated include ethyl diazoacetate, tris(trifluoromethylphosphine, heptafluorobutyrate, 3-fluoro-2-propynenitrite, 4-(2-propenylphenol, and eugenol. The results of this study could lead to the development of novel therapeutic agents capable of dealing with specific diseases that either have weakened reaction or are currently not responsive to existing drugs.

  13. A simple analytical platform based on thin-layer chromatography coupled with paper-based analytical device for determination of total capsaicinoids in chilli samples.

    Science.gov (United States)

    Dawan, Phanphruk; Satarpai, Thiphol; Tuchinda, Patoomratana; Shiowatana, Juwadee; Siripinyanond, Atitaya

    2017-01-01

    A new analytical platform based on the use of thin-layer chromatography (TLC) coupled with paper-based analytical device (PAD) was developed for the determination of total capsaicinoids in chilli samples. This newly developed TLC-PAD is simple and low-cost without any requirement of special instrument or skillful person. The analysis consisted of two steps, i.e., extraction of capsaicinoids from chilli samples by using ethanol as solvent and separation of capsaicinoids by thin-layer chromatography (TLC) and elution of capsaicinoids from the TLC plate with in situ colorimetric detection of capsaicinoids on the PAD. For colorimetric detection, Folin-Ciocalteu reagent was used to detect phenolic functional group of capsaicinoids yielding the blue color. The blue color on the PAD was imaged by a scanner followed by evaluation of its grayscale intensity value by ImageJ program. This newly developed TLC-PAD method provided a linear range from 50 to 1000mgL-1 capsaicinoids with the limit of detection as low as 50mgL-1 capsaicinoids. The proposed method was applied to determine capsaicinoids in dried chilli and seasoning powder samples and the results were in good agreement with those obtained by HPLC method. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Análise de resíduos de pesticidas em tomates por cromatografia em camada delgada Analysis of residue pesticide in tomatoes by thin layer chromatography

    Directory of Open Access Journals (Sweden)

    Solange Leite Moraes

    2002-05-01

    Full Text Available Pesticide residues are determined by thin layer chromatography (TLC using the Hill reaction as a detection method. Tomatoes samples without pesticide were fortified with atrazine, diuron, chloroxuron and metribuzin, and were applyed in silica gel plates with the help of a microsyringe. The pesticides were elued with ethyl acetate. There was no need of cleaning up because no interference was noticed. After the revelation of the plates, the diameters of the spots were measure by using a rule. The range of the determined concentration for all the pesticides was from 0.1 to1.0 ng/muL. The results obtained through TLC can be used for semi-quantitative analysis.The results obtained were compared to gas and liquid chromatography, showing good agreement between both techniques.

  15. High-performance thin layer chromatography method for quantitative determination of four major anthraquinone derivatives in Rheum emodi.

    Science.gov (United States)

    Singh, Narendra P; Gupta, Ajai P; Sinha, Arun K; Ahuja, Paramvir S

    2005-06-10

    A high-performance thin layer chromatographic (HPTLC) method for the rapid and simple quantification of the four major anthraquinone derivatives i.e. physcion, chrysophanol, emodin and chrysophanol glycoside in Rheum emodi is described. HPTLC of anthraquinone derivatives was performed on pre-coated RP-18 F254S HPTLC plates. For achieving good separation, the mobile phase of methanol-water-formic acid (80:19:1, v/v/v) was used. The densitometric determination of anthraquinone derivatives was carried out at 445 nm in reflection/absorption mode. The calibration curves were linear in the range of 20-100 ng for physcion, 80-400 ng for chrysophanol and emodin, and 200-1000 ng for chrysophanol glycoside. The method was found to be reproducible and convenient for quantitative analysis of anthraquinone derivatives in the methanolic extract of rhizomes of R. emodi collected from three different locations of Western Himalaya, India.

  16. Hydrocarbon type analysis by thin-layer chromatography with flame-ionization detection: vacuum gas oils, heavy feeds, and hydroprocessed products.

    Science.gov (United States)

    Barman, Bhajendra N

    2004-03-01

    Thin-layer chromatography with flame-ionization detection (TLC-FID) provides quantitative hydrocarbon type data as well as distribution of aromatics by ring number. This method has been applied to obtain amounts of saturates, aromatics, and polars in heavy oil distillates such as light vacuum gas oils and heavy vacuum gas oils derived from different crude sources. TLC-FID chromatograms and resultant quantitative hydrocarbon type data show that these distillates vary markedly in aromatic contents and aromatic ring types. Similar observations are made with several fluid catalytic cracking feeds. Effects of process parameters such as operating pressure and temperature on hydroconversion of aromatics and polars from a heavy oil are assessed by TLC-FID. It has been demonstrated that there is a preferential reduction of higher polycyclic aromatic hydrocarbons and polars with an increase of both hydrogen partial pressure and reactor temperature.

  17. Composite glycerol/graphite/aromatic acid matrices for thin-layer chromatography/matrix-assisted laser desorption/ionization mass spectrometry of heterocyclic compounds.

    Science.gov (United States)

    Esparza, Cesar; Borisov, R S; Varlamov, A V; Zaikin, V G

    2016-10-28

    New composite matrices have been suggested for the analysis of mixtures of different synthetic organic compounds (N-containing heterocycles and erectile dysfunction drugs) by thin layer chromatography/matrix-assisted laser desorption ionization time-of-flight mass spectrometry (TLC/MALDI-TOF). Different mixtures of classical MALDI matrices and graphite particles dispersed in glycerol were used for the registration of MALDI mass spectra directly from TLC plates after analytes separation. In most of cases, the mass spectra possessed [M+H](+) ions; however, for some analytes only [M+Na](+) and [M+K](+) ions were observed. These ions have been used to generate visualized TLC chromatograms. The described approach increases the desorption/ionization efficiencies of analytes separated by TLC, prevent spot blurring, simplifies and decrease time for sample preparation. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Quantification of Sunscreen Benzophenone-4 in Hair Shampoos by Hydrophilic Interactions Thin-Layer Chromatography/Densitometry or Derivative UV Spectrophotometry.

    Science.gov (United States)

    Sobańska, Anna W; Kałębasiak, Katarzyna; Pyzowski, Jarosław; Brzezińska, Elżbieta

    2015-01-01

    Benzophenone-4 (BZ4) was separated from surfactants, dyes, preservatives, and other components of hair shampoos by thin-layer chromatography on silica gel 60 stationary phase, with ethyl acetate-ethanol-water-pH 6 phosphate buffer (15 : 7 : 5 : 1 v/v/v/v) as mobile phase. Densitometry scanning of chromatograms was performed at 285 nm. The densitometric calibration curve for BZ4 was nonlinear (second-degree polynomial), with R > 0.999. The limits of detection and quantification were ca. 0.03 and ca. 0.1 μg spot(-1), respectively. The results obtained by HPTLC-densitometry were compared to those obtained by zero and 2nd derivative UV spectrophotometry. In the case of spectrophotometric methods, calibration curves were linear with R > 0.9998. The chromatographic method was fully validated.

  19. Quantification of Sunscreen Benzophenone-4 in Hair Shampoos by Hydrophilic Interactions Thin-Layer Chromatography/Densitometry or Derivative UV Spectrophotometry

    Directory of Open Access Journals (Sweden)

    Anna W. Sobańska

    2015-01-01

    Full Text Available Benzophenone-4 (BZ4 was separated from surfactants, dyes, preservatives, and other components of hair shampoos by thin-layer chromatography on silica gel 60 stationary phase, with ethyl acetate-ethanol-water-pH 6 phosphate buffer (15 : 7 : 5 : 1 v/v/v/v as mobile phase. Densitometry scanning of chromatograms was performed at 285 nm. The densitometric calibration curve for BZ4 was nonlinear (second-degree polynomial, with R>0.999. The limits of detection and quantification were ca. 0.03 and ca. 0.1 μg spot−1, respectively. The results obtained by HPTLC-densitometry were compared to those obtained by zero and 2nd derivative UV spectrophotometry. In the case of spectrophotometric methods, calibration curves were linear with R>0.9998. The chromatographic method was fully validated.

  20. Coupling thin-layer chromatography with vibrational cooling matrix-assisted laser desorption/ionization Fourier transform mass spectrometry for the analysis of ganglioside mixtures.

    Science.gov (United States)

    Ivleva, Vera B; Elkin, Yuri N; Budnik, Bogdan A; Moyer, Susanne C; O'Connor, Peter B; Costello, Catherine E

    2004-11-01

    Thin-layer chromatography (TLC), which is widely used for separation of glycolipids, oligosaccharides, lipids, and compounds of environmental and pharmaceutical interest, can be readily coupled to matrix-assisted laser desorption/ionization (MALDI) time-of-flight mass spectrometers, but this arrangement usually compromises mass spectral resolution due to the irregularity of the TLC surface. However, TLC can be coupled to an external ion source MALDI-Fourier transform (FT) MS instrument without compromising mass accuracy and resolution of the spectra. Furthermore, when the FTMS has a vibrationally cooled MALDI ion source, fragile glycolipids can be desorbed from TLC plates without fragmentation, even to the point that desorption of intact molecules from "hot"matrixes such as alpha-cyano-4-hydroxycinnamic acid is possible. In this work, whole brain gangliosides are separated using TLC; the TLC plates are attached directly to the MALDI target, where the gangliosides are desorbed, ionized, and detected in the FTMS with >70 000 resolving power.

  1. Chemical variability along the value chains of turmeric (Curcuma longa): a comparison of nuclear magnetic resonance spectroscopy and high performance thin layer chromatography.

    Science.gov (United States)

    Booker, Anthony; Frommenwiler, Debora; Johnston, Deborah; Umealajekwu, Chinenye; Reich, Eike; Heinrich, Michael

    2014-03-14

    Herbal medicine value chains have generally been overlooked compared with food commodities. Not surprisingly, revenue generation tends to be weighted towards the end of the chain and consequently the farmers and producers are the lowest paid beneficiaries. Value chains have an impact both on the livelihood of producers and on the composition and quality of products commonly sold locally and globally and consequently on the consumers. In order to understand the impact of value chains on the composition of products, we studied the production conditions for turmeric (Curcuma longa) and the metabolomic composition of products derived from it. We aimed at integrating these two components in order to gain a better understanding of the effect of different value chains on the livelihoods of some producers. This interdisciplinary project uses a mixed methods approach. Case studies were undertaken on two separate sites in India. Data was initially gathered on herbal medicine value chains by means of semi-structured interviews and non-participant observations. Samples were collected from locations in India, Europe and the USA and analysed using (1)H NMR spectroscopy coupled with multivariate analysis software and with high performance thin layer chromatography (HPTLC). We investigate medicinal plant value chains and interpret the impact different value chains have on some aspects of the livelihoods of producers in India and, for the first time, analytically assess the chemical variability and quality implications that different value chains may have on the products available to end users in Europe. There are benefits to farmers that belonged to an integrated chain and the resulting products were subject to a higher standard of processing and storage. By using analytical methods, including HPTLC and (1)H NMR spectroscopy, it has been possible to correlate some variations in product composition for selected producers and identify strengths and weaknesses of some types of value

  2. Monitoring of monooctanoylphosphatidylcholine synthesis by enzymatic acidolysis between soybean phosphatidylcholine and caprylic acid by thin-layer chromatography with a flame ionization detector.

    Science.gov (United States)

    Vikbjerg, Anders F; Mu, Huiling; Xu, Xuebing

    2005-05-18

    Thin-layer chromatography with a flame ionization detector (TLC-FID) was used for monitoring the production of structured phospholipids (ML type: L, long-chain fatty acids; M, medium-chain fatty acids) by enzyme-catalyzed acidolysis between soybean phosphatidylcholine (PC) and caprylic acid. It was found that the structured PC fractionated into two to three distinct bands on both plate thin-layer chromatography (TLC) and Chromarod TLC. These three bands represented PC of the LL type, ML type, and MM type, respectively. The TLC-FID method was applied in the present study to examine the influence of enzyme dosage, reaction temperature, solvent amount, reaction time, and substrate ratio (caprylic acid/PC, mol/mol) on formation of ML-type PC in a batch reactor with Thermomyces lanuginosa lipase as the catalyst. The formation of ML-type PC was dependent on all parameters examined except for the substrate ratio. The ML-type PC content increased with increasing enzyme dosage, reaction temperature, solvent amount, and reaction time. The substrate ratio had no significant effect on the formation of ML-type PC within the tested range (3-15 mol/mol). The formation of MM-type PC was observed in some experiments, indicating that acyl migration is taking place during reaction since the lipase is claimed to be 1,3-specific. The TLC-FID method offers a simple and cheap technique for elucidation of product and byproduct formation during enzyme-catalyzed reactions for production of phospholipids containing mixtures of long- and medium-chain fatty acids.

  3. Coupling of column liquid chromatography and surface-enhanced resonance Raman spectroscopy via a thin-layer chromatographic plate.

    NARCIS (Netherlands)

    Coulter, S.K.; Gooijer, C.; Velthorst, N.H.; Brinkman, U.A.T.; Somsen, G.W.

    1997-01-01

    Surface-enhanced resonance Raman (SERR) spectroscopy was used to characterize compounds separated by column liquid chromatography (LC). Three percent of the effluent from a conventional-size LC column were immobilized on a moving thinlayer chromatography (TLC) plate using a spray-jet

  4. Use of thin layer chromatography for the determination of radiochemical purity of radiopharmaceuticals in nuclear medicine services of Paraiba and Rio Grande do Norte, Brazil; Utilizacao da cromatografia em camada delgada para determinacao da pureza radioquimica de radiofarmacos em servicos de medicina nuclear da Paraiba e Rio Grande do Norte, Brasil

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, W.G.; Santos, P.A.L.; Lima, F.R.A. [Universidade Federal de Pernambuco (UFPE), Recife, PE (Brazil). Programa de Pos-Graduacao em Tecnologia Energetica; Lima, F.F., E-mail: wellington.gandrade@gmail.com [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

    2012-07-01

    The paper chromatography and the thin layer chromatography are separation techniques in which the radioactive components migrate because of their affinity with the eluent (mobile phase) or stationary phase, respectively. In radiopharmaceuticals labeled with {sup 99m}Tc, besides its own radiopharmaceutical, {sup 99m}TcO{sup 4-} free and TcO{sub 2} can be identified and quantified. The evaluation of radiochemical purity of radiopharmaceuticals is essential to produce images free of artifacts as well as avoid unnecessary absorbed dose to the patient. Once they are managed in humans it is important and necessary that they undergo to strict quality control. Because of this, ANVISA in its 'Resolucao da Diretoria Colegiada (RDC) 38 of June 4th, 2008 states the obligation of performing a minimum of tests in nuclear medicine services routine prior to human administration. This work evaluated, by the method of thin layer chromatography (TLC), radiochemical purity, determined the pH of the radiopharmaceutical DEXTRAN- 500, DMSA, DTPA, PHYTATE, MDP, MIBI and Sn-Col used in nuclear medicine services in the states of Paraiba and Rio Grande do Norte - Brazil. The results show that the use of thin layer chromatography (TLC) as a standard method in routine of nuclear medicine services is possible, because it provides important data for the evaluation of radiochemical purity, allowing the exclusion of a radiopharmaceutical poorly marked. (author)

  5. Identification of Ginkgo biloba supplements adulteration using high performance thin layer chromatography and ultra high performance liquid chromatography-diode array detector-quadrupole time of flight-mass spectrometry.

    Science.gov (United States)

    Avula, Bharathi; Sagi, Satyanarayanaraju; Gafner, Stefan; Upton, Roy; Wang, Yan-Hong; Wang, Mei; Khan, Ikhlas A

    2015-10-01

    Ginkgo biloba is one of the most widely sold herbal supplements and medicines in the world. Its popularity stems from having a positive effect on memory and the circulatory system in clinical studies. As ginkgo popularity increased, non-proprietary extracts were introduced claiming to have a similar phytochemical profile as the clinically tested extracts. The standardized commercial extracts of G. biloba leaf used in ginkgo supplements contain not less than 6% sesquiterpene lactones and 24% flavonol glycosides. While sesquiterpene lactones are unique constituents of ginkgo leaf, the flavonol glycosides are found in many other botanical extracts. Being a high value botanical, low quality ginkgo extracts may be subjected to adulteration with flavonoids to meet the requirement of 24% flavonol glycosides. Chemical analysis by ultra high performance liquid chromatography-mass spectrometry revealed that adulteration of ginkgo leaf extracts in many of these products is common, the naturally flavonol glycoside-rich extract being spiked with pure flavonoids or extracts made from another flavonoid-rich material, such as the fruit/flower of Japanese sophora (Styphnolobium japonicum), which also contains the isoflavone genistein. Recently, genistein has been proposed as an analytical marker for the detection of adulteration of ginkgo extracts with S. japonicum. This study confirms that botanically authenticated G. biloba leaf and extracts made therefrom do not contain genistein, and the presence of which even in trace amounts is suggestive of adulteration. In addition to the mass spectrometric approach, a high performance thin layer chromatography method was developed as a fast and economic method for chemical fingerprint analysis of ginkgo samples.

  6. Chromatography.

    Science.gov (United States)

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  7. Stability-indicating reversed-phase high-performance thin-layer chromatography/densitometry estimation of lafutidine in bulk and tablets

    Directory of Open Access Journals (Sweden)

    Prajapati Nitin D.

    2013-01-01

    Full Text Available Lafutidine (LTD is a histamine H2 receptor antagonist, with anti-ulcer and mucosal protective activity. A sensitive and selective stability-indicating reversed- phase high -performance thin-layer chromatography (RP-HPTLC/Densitometry method is suggested for the determination of LTD in the presence of its acid, alkaline, oxidative and dry heat degradation products. Stress testing of LTD was done according to the International Conference on Harmonization (ICH guidelines in order to validate the stability-indicating power of the analytical procedures. Stress testing demonstrated that LTD underwent acid, alkaline, oxidative and dry heat degradation; on the other hand, it showed stability towards neutral and photo degradation. Chromatography was performed on aluminum-backed silica gel 60 RP-18 F254 S plates with Methanol: Water: Triethylamine 8: 2: 0.5 (v/v as mobile phase. Densitometric scanning was performed at 276 nm. The system gave compact bands for LTD (Rf 0.67 ± 0.02. Linear regression analysis data for the calibration plots discovered a good linear relationship with r2 > 0.99 in the working concentration range 500 to 3000 ng per band. The limits of detection and quantification were 23.51 ng and 71.26 ng, respectively. The developed method can routinely be used for analysis of LTD in bulk and pharmaceutical formulations.

  8. Characterization of Mycobacterium paratuberculosis by gas-liquid and thin-layer chromatography and rapid demonstration of mycobactin dependence using radiometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Damato, J.J.; Knisley, C.; Collins, M.T.

    1987-12-01

    Thirty-six Mycobacterium paratuberculosis isolates of bovine, caprine, and ovine origins were evaluated by using gas-liquid chromatography (GLC), thin-layer chromatography (TLC), and BACTEC 7H12 Middlebrook TB medium in an effort to more rapidly differentiate this group of organisms from other mycobacteria. Bacterial suspensions (0.1 ml) were inoculated by syringe into 7H12 broth containing 2 micrograms of mycobactin P per ml and control broth without mycobactin P. Cultures were incubated at 37/sup 0/C and read daily with a BACTEC Model 301. After 8 days of incubation, the growth index readings for the test broths containing mycobactin P were twice those of the control broths without mycobactin P. Sixty-five isolates of mycobacteria other than M. paratuberculosis were also examined. No difference was noted between the growth index readings of control and mycobactin-containing broths. Except for Mycobacterium avium-Mycobacterium intracellulare, TLC studies differentiated M. paratuberculosis from the other mycobacterial species tested. The GLC data reveal that all M. paratuberculosis isolates had a distinctive peak (14A) which was not found among M. avium-M. intracellulare complex organisms. These data indicate that 7H12 radiometric broth was able to rapidly demonstrate the mycobactin dependence of M. paratuberculosis and GLC and TLC procedures were capable of rapidly differentiating this organism from the other mycobacteria studied.

  9. Analysis of Bioactive Components of Oilseed Cakes by High-Performance Thin-Layer Chromatography-(Bioassay Combined with Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Sue-Siang Teh

    2015-03-01

    Full Text Available Hemp, flax and canola seed cakes are byproducts of the plant oil extraction industry that have not received much attention in terms of their potential use for human food instead of animal feed. Thus, the bioactivity profiling of these oilseed cakes is of interest. For their effect-directed analysis, planar chromatography was combined with several (bioassays, namely 2,2-diphenyl-1-picrylhydrazyl scavenging, acetylcholine esterase inhibition, planar yeast estrogen screen, antimicrobial Bacillus subtilis and Aliivibrio fischeri assays. The streamlined high-performance thin-layer chromatography (HPTLC-bioassay method allowed the discovery of previously unknown bioactive compounds present in these oilseed cake extracts. In contrast to target analysis, the direct link to the effective compounds allowed comprehensive information with regard to selected effects. HPTLC-electrospray ionization-mass spectrometry via the elution-head based TLC-MS Interface was used for a first characterization of the unknown effective compounds. The demonstrated bioactivity profiling on the feed/food intake side may guide the isolation of active compounds for production of functional food or for justified motivation of functional feed/food supplements.

  10. Prediction of the lipophilicity of nine new synthesized selenazoly and three aroyl-hydrazinoselenazoles derivatives by reversed-phase high performance thin-layer chromatography.

    Science.gov (United States)

    Cozma, A; Zaharia, V; Ignat, A; Gocan, S; Grinberg, N

    2012-03-01

    Using reversed-phase high-performance thin-layer chromatography and a methanol-water mixture as the mobile phase, the lipophilicity of 12 new synthesized derivatives is studied. The first eight compounds have as a basic chemical structure aryliden-hydrazino-selenazoles, and the second group of the three compounds belongs to aroyl-hydrazinoselenazoles. The linear correlation between R(Mw) and the methanol-water ratios showed high values for the correlation coefficient. The chromatographic hydrophobic index is determined by using the ratio -R(Mw)/S, and the obtained values ranged between 99 and 73. A good linear correlation is obtained between R(Mw) and the slope. The log P values are calculated using ACD/Labs Software. The matrices are formed with R(Mw) and log P and are subjected to a principal component analysis (PCA). The best way to extract information from PCA is graphically, by plotting the obtained matrices. By analyzing the scores, the compounds can be grouped as follows: a group containing nine compounds, and a second one containing three compounds. Each group of compounds has the same basic chemical structure.

  11. Thin layer chromatography-spray mass spectrometry: a method for easy identification of synthesis products and UV filters from TLC aluminum foils.

    Science.gov (United States)

    Himmelsbach, Markus; Waser, Mario; Klampfl, Christian W

    2014-06-01

    A straightforward procedure for direct mass spectrometric (MS) analysis of spots from thin layer chromatography (TLC) plates, without the need of an external ion source, was developed using the aluminum plate backing as spray tip. The spots were cut out shaped as a tip with a 60° angle, mounted in front of the MS orifice, and after addition of a spray solvent spectra were obtained immediately. A high-resolution time-of-flight MS was used since the method is of particular interest for rapid identification or confirmation of spots from TLC plates. The practical benefits of this technique were demonstrated by detection of by-products of organic reactions, by identification of degradation products, and by accurate confirmation of spots when UV filters in sunscreens were analyzed by TLC. Employing the described method TLC spots can be evaluated fast without the need of an external ion source or devices for analyte transfer from TLC to MS, only a basic MS instrument and a high-voltage power supply is required.

  12. Algerian mint species: high performance thin layer chromatography quantitative determination of rosmarinic acid and in vitro inhibitory effects on linoleic acid peroxidation

    Directory of Open Access Journals (Sweden)

    Brahmi Fatiha

    2014-12-01

    Full Text Available Objective: To determine the quantitative paremeters of rosmarinic acid in Algerian mints, Mentha spicata L. (M. spicata, Mentha pulegium L. and Mentha rotundifolia (L. Huds by high performance thin layer chromatography (HPTLC-densitometric method and screen the effects of these plant extracts on linoleic acid peroxidation. Methods: The analyses were performed on HPTLC silica gel 60 F254 plates with chloroform: acetone: formic acid (75:16.5:8.5, v/v as the mobile phase. Rosmarinic acid was determined in UV at 365 nm and fluorescence at λexc 325 nm with a 550 nm filter, respectively. The effects of plants extracts on linoleic acid peroxidation were measured by an indirect in vitro colorimetric method. Results: Chromatographic resolution permitted reliable quantification in both measurement modes and calibration curves were linear in a range of 150-1 000 ng/spot. M. spicata was found to contain significantly higher concentrations of rosmarinic acid. The densitometric quantification allowed the analysis of many samples in a short time with reasonable precision (total precision for Mentha spp extracts, 5.1% and 5.8% for UV and fluorescence detection, respectively. The HPTLC data, allied to assays of linoleic acid peroxidation prevention, suggested the potential of M. spicata (52% Trolox® equivalents as a natural source for inhibitors of lipid peroxidation. Conclusions: Densitometry can be used for routine determination and quality control of rosmarinic acid in herbal and formulations containing Mentha species.

  13. Effect of hydrolysis on the yield of hederagenin and High-performance thin-layer chromatography densitometric quantification of hederagenin in fruit pericarp of Sapindus spp.

    Science.gov (United States)

    Kalola, Jyoti; Anandjiwala, Sheetal; Srinivasa, Honnegowda; Rajani, Mandapati

    2008-01-01

    Fruit pericarp of Sapindus species are reported to contain glycosides with hederagenin as an aglycone. To free the aglycone from the glycosides, they need to be hydrolyzed, and the commonly used method is hydrolysis with either hydrochloric or sulfuric acid. In the present work, we studied the effect of hydrolysis on the yield of hederagenin from the fruit pericarp of 3 species of Sapindus, viz., S. mukorossi, S. laurifolius, and S. emarginatus. A high-performance thin-layer chromatography densitometric method for the quantification of hederagenin was developed and validated. It involved automated application of samples as bands onto silica gel 60F254 plates, development with toluene-ethyl acetate-formic acid (7 + 3 + 5, v/v/v) mobile phase, detection with anisaldehyde-sulfuric acid reagent, and scanning at 595 nm. The yield of hederagenin ranged from 0.035 to 1.29% (w/w) with different methods of hydrolysis. Hydrolysis with 3.5 M aqueous sulfuric acid under reflux for 6 h gave the maximum yield of hederagenin in all 3 species, with the highest amount in S. emarginatus (1.29%, w/w).

  14. Direct analysis of pharmaceutical formulations from non-bonded reversed-phase thin-layer chromatography plates by desorption electrospray ionisation ion mobility mass spectrometry.

    Science.gov (United States)

    Harry, Emma L; Reynolds, James C; Bristow, Anthony W T; Wilson, Ian D; Creaser, Colin S

    2009-09-01

    The direct analysis of pharmaceutical formulations and active ingredients from non-bonded reversed-phase thin layer chromatography (RP-TLC) plates by desorption electrospray ionisation (DESI) combined with ion mobility mass spectrometry (IM-MS) is reported. The analysis of formulations containing analgesic (paracetamol), decongestant (ephedrine), opiate (codeine) and stimulant (caffeine) active pharmaceutical ingredients is described, with and without chromatographic development to separate the active ingredients from the excipient formulation. Selectivity was enhanced by combining ion mobility and mass spectrometry to characterise the desorbed gas-phase analyte ions on the basis of mass-to-charge ratio (m/z) and gas-phase ion mobility (drift time). The solvent composition of the DESI spray using a step gradient was varied to optimise the desorption of active pharmaceutical ingredients from the RP-TLC plates. The combined RP-TLC/DESI-IM-MS approach has potential as a rapid and selective technique for pharmaceutical analysis by orthogonal gas-phase electrophoretic and mass-to-charge separation. Copyright (c) 2009 John Wiley & Sons, Ltd.

  15. Construction of a supercritical fluid extraction (SFE equipment: validation using annatto and fennel and extract analysis by thin layer chromatography coupled to image

    Directory of Open Access Journals (Sweden)

    Júlio Cezar Flores JOHNER

    2016-01-01

    Full Text Available Abstract The present work describes setting up a laboratory unit for supercritical fluid extraction. In addition to its construction, a survey of cost was done to compare the cost of the homemade unit with that of commercial units. The equipment was validated using an extraction of annatto seeds’ oil, and the extraction and fractionation of fennel oil were used to validate the two separators; for both systems, the solvent was carbon dioxide. The chemical profiles of annatto and fennel extracts were assessed using thin layer chromatography; the images of the chromatographic plates were processed using the free ImageJ software. The cost survey showed that the homemade equipment has a very low cost (~US$ 16,000 compared to commercial equipment. The extraction curves of annatto were similar to those obtained in the literature (yield of 3.8% oil. The separators were validated, producing both a 2.5% fraction of fennel seed extract rich in essential oils and another extract fraction composed mainly of oleoresins. The ImageJ software proved to be a low-cost tool for obtaining an initial evaluation of the chemical profile of the extracts.

  16. High-performance thin-layer chromatography screening of multi class antibiotics in animal food by bioluminescent bioautography and electrospray ionization mass spectrometry.

    Science.gov (United States)

    Chen, Yisheng; Schwack, Wolfgang

    2014-08-22

    The world-wide usage and partly abuse of veterinary antibiotics resulted in a pressing need to control residues in animal-derived foods. Large-scale screening for residues of antibiotics is typically performed by microbial agar diffusion tests. This work employing high-performance thin-layer chromatography (HPTLC) combined with bioautography and electrospray ionization mass spectrometry introduces a rapid and efficient method for a multi-class screening of antibiotic residues. The viability of the bioluminescent bacterium Aliivibrio fischeri to the studied antibiotics (16 species of 5 groups) was optimized on amino plates, enabling detection sensitivity down to the strictest maximum residue limits. The HPTLC method was developed not to separate the individual antibiotics, but for cleanup of sample extracts. The studied antibiotics either remained at the start zones (tetracyclines, aminoglycosides, fluoroquinolones, and macrolides) or migrated into the front (amphenicols), while interfering co-extracted matrix compounds were dispersed at hRf 20-80. Only after a few hours, the multi-sample plate image clearly revealed the presence or absence of antibiotic residues. Moreover, molecular information as to the suspected findings was rapidly achieved by HPTLC-mass spectrometry. Showing remarkable sensitivity and matrix-tolerance, the established method was successfully applied to milk and kidney samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Qualitative and quantitative high performance thin layer chromatography analysis of Calendula officinalis using high resolution plate imaging and artificial neural network data modelling.

    Science.gov (United States)

    Agatonovic-Kustrin, S; Loescher, Christine M

    2013-10-10

    Calendula officinalis, commonly known Marigold, has been traditionally used for its anti-inflammatory effects. The aim of this study was to investigate the capacity of an artificial neural network (ANN) to analyse thin layer chromatography (TLC) chromatograms as fingerprint patterns for quantitative estimation of chlorogenic acid, caffeic acid and rutin in Calendula plant extracts. By applying samples with different weight ratios of marker compounds to the system, a database of chromatograms was constructed. A hundred and one signal intensities in each of the HPTLC chromatograms were correlated to the amounts of applied chlorogenic acid, caffeic acid, and rutin using an ANN. The developed ANN correlation was used to quantify the amounts of 3 marker compounds in calendula plant extracts. The minimum quantifiable level (MQL) of 610, 190 and 940 ng and the limit of detection (LD) of 183, 57 and 282 ng were established for chlorogenic, caffeic acid and rutin, respectively. A novel method for quality control of herbal products, based on HPTLC separation, high resolution digital plate imaging and ANN data analysis has been developed. The proposed method can be adopted for routine evaluation of the phytochemical variability in calendula extracts. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Detection and Estimation of alpha-Amyrin, beta-Sitosterol, Lupeol, and n-Triacontane in Two Medicinal Plants by High Performance Thin Layer Chromatography

    Directory of Open Access Journals (Sweden)

    Saikat S. Mallick

    2014-01-01

    Full Text Available A normal phase high performance thin layer chromatography (HPTLC method has been developed and validated for simultaneous estimation of four components, namely, alpha-amyrin, beta-sitosterol, lupeol, and n-triacontane from two medicinally important plants, Leptadenia reticulata Wight & Arn. and Pluchea lanceolata (DC. CB. Clarke. In Ayurveda, both plants have been reported to possess immunomodulatory activity. Chromatographic separation of the four components from the methanolic extracts of whole plant powders of Leptadenia reticulata Wight & Arn. and Pluchea lanceolata (DC. CB. Clarke. was performed on TLC aluminium plates precoated with silica gel 60F254 using a suitable mobile phase. The densitometric scanning was done after derivatization at λ = 580 nm for α-amyrin, β-sitosterol, and lupeol, and at 366 nm for n-triacontane. The developed HPTLC method has been validated and used for simultaneous quantitation of the four components from the methanolic extracts of whole plant powders of Leptadenia reticulata Wight & Arn. and Pluchea lanceolata (DC. CB. Clarke. The developed HPTLC method is simple, rapid, and precise and can be used for routine quality control.

  19. Application of thin-layer chromatography with fluorescence scanning densitometry for analysing saturates in heavy liquids derived from co-pyrolysis of biomass and plastics

    Energy Technology Data Exchange (ETDEWEB)

    Cebolla, V.L. [Consejo Superior de Investigaciones Cientificas (CSIC), Instituto de Carboquimica, Zaragoza (Spain); Matt, M. [Institute of Chemistry and Chemical Technology, Krasnoyarsk (Russian Federation). Siberian Branch of Russian Academy of Sciences; Membrado, L. [Universite de Metz, Saint-Avold (FR). Laboratoire de Chimie et Applications] [and others

    2002-01-01

    Two alternative methods, based on Thin-Layer Chromatography (TLC) with Fluorescence Scanning Densitometry have been developed for characterization of heavy liquids from copyrolysis of different kinds of biomass and plastics in autoclaves under inert atmosphere. A conventional TLC system, which includes a vertical developing tank, and a High Performance TLC (HPTLC) system, with a horizontal developing chamber and the use of HPTLC plates, have been used. The analytical method involves in both cases the measurement of two chromatograms per sample: the first, on a silica gel berberine-impregnated plate, for detection of saturates using the phenomenon of berberine-induced fluorescence; and the second, on a silica gel plate, for detection of aromatic-polars and polars, by native fluorescence. Although the HPTLC system is more sensitive and faster, both techniques represent an improvement with regard to current methods for analyzing these kinds of products. However their application depends on the particular solubility of each sample and on its slope of the fluorescent response-sample load regression. (orig.)

  20. High-performance thin-layer chromatography HPTLC-direct bioautography as a method of choice for alpha-amylase and antioxidant activity evaluation in marine algae.

    Science.gov (United States)

    Agatonovic-Kustrin, Snezana; Morton, David W

    2017-12-29

    High-Performance Thin-layer chromatography (HPTLC) combined with DPPH free radical method and α-amylase bioassay was used to compare antioxidant and antidiabetic activities in ethanol and ethyl acetate extracts from 10 marine macroalgae species (3 Chlorophyta, 4 Phaeophyta and 3 Rhodophyta) from Blue Lagoon beach (Malaysia). Samples were also evaluated for their phenolic and stigmasterol content. On average, higher antioxidant activity was observed in the ethyl acetate extracts (55.1mg/100g gallic acid equivalents (GAE) compared to 35.0mg/100g GAE) while, as expected, phenolic content was higher in ethanol extracts (330.5mg/100g GAE compared to 289.5mg/100g GAE). Amounts of fucoxanthin, stigmasterol and α-amylase inhibitory activities were higher in ethyl acetate extracts. Higher enzyme inhibition is therefore related to higher concentrations of triterpenes and phytosterols (Note: these compounds are more soluble in ethyl acetate). Ethyl acetate extracts from Caulerpa racemosa and Padina minor, had the highest α-amylase inhibitory activity, and also showed moderately high antioxidant activities, stigmasterol content and polyphenolic content. Caulerpa racemose, being green algae, does not contain fucoxanthin, while Padina minor, being brown algae, contains high amounts of fucoxanthin. Therefore, it is very unlikely that fucoxanthin contributes to α-amylase inhibitory activity as previously reported. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

  1. Analysis of brain lipids by directly coupled matrix-assisted laser desorption ionization time-of-flight mass spectrometry and high-performance thin-layer chromatography.

    Science.gov (United States)

    Fuchs, Beate; Nimptsch, Ariane; Suss, Rosmarie; Schiller, Jürgen

    2008-01-01

    Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS) is a soft ionization MS technique providing only minor fragmentation of the analyte. Therefore, the method is basically suitable for mixture analysis, although the ion yields strongly depend on the basicity/acidity of the analyte in relation to the applied matrix. Accordingly, less sensitively detectable compounds may be suppressed by more sensitively detectable compounds. Thus, separation of the mixture into the individual compounds is normally indispensable. This paper demonstrates the capabilities and limitations of a direct, simple, and inexpensive MALDI-high-performance thin-layer chromatography (HPTLC) coupling for the analysis of a crude lipid extract from porcine brain. Brain lipids were chosen because they represent a rather complex mixture and are of currently significant research interest. It was found that normal-phase HPTLC-separated lipids can be easily characterized by direct MALDI-TOF-MS analysis with sufficient resolution to allow the assignment of virtually all lipid classes, even rather minor species such as phosphorylated phosphoinositides or complex glycolipids as gangliosides. Advantages and disadvantages of this approach are discussed.

  2. Development of an efficient high-performance thin layer chromatography method for determination of jasmonic acid in leaf tissue of Stevia rebaudiana (Bertoni) Bertoni.

    Science.gov (United States)

    Kilam, Divya; Saifi, M; Agnihotri, A; Abdin, M Z

    2017-07-01

    Determination of endogenous levels of jasmonic acid (JA) is essential, as it plays a pivotal role in the physiological processes during a plant's life cycle. A high performance thin layer chromatography (HPTLC) method was developed for the detection and quantification of JA in leaf extracts of medicinal plant, Stevia rebaudiana (Bertoni) Bertoni. The separation was achieved using the solvents ethyl acetate-benzene (1:1, v/v) as the mobile phase, followed by scanning and quantification at 295 nm. Densitometric analysis of leaf extract resulted in compact spots for JA at Rf = 0.45 ± 0.02. The linear regression analysis showed good relationship with r value. The recovery rate of JA indicated good reproducibility and repeatability of the assay. The statistical analysis proved the reproducibility of the method; therefore, it can be employed for routine quantification of JA in different tissue samples of S. rebaudiana and may also be extrapolated to other biological samples.

  3. A new high-performance thin layer chromatography-based assay of detergents and surfactants commonly used in membrane protein studies.

    Science.gov (United States)

    Barret, Laurie-Anne; Polidori, Ange; Bonneté, Françoise; Bernard-Savary, Pierre; Jungas, Colette

    2013-03-15

    The hydrophobic nature of membrane proteins (MPs) necessitates the use of detergents for their extraction, solubilization and purification. Because the concentration of amphiphiles is crucial in the crystallization process, detergent quantification is essential to routine analysis. Here we describe a quantitative high-performance thin-layer chromatography (HPTLC) method we developed for the detection of small quantities of detergent bound to solubilized MPs. After optimization of aqueous deposit conditions, we show that most detergents widely used in membrane protein crystallography display distinctive mobilities in a mixture of dichloromethane, methanol and acetic acid 32:7.6:0.4 (v/v/v). Migration and derivatization conditions were optimized with n-dodecyl-β-D-maltoside (DDM), the most popular detergent for membrane protein crystallization. A linear calibration curve very well fits our data from 0.1 to 1.6 μg of DDM in water with a limit of detection of 0.05 μg. This limit of detection is the best achieved to date for a routine detergent assay, being not modified by the addition of NaCl, commonly used in protein buffers. With these chromatographic conditions, no prior treatment is required to assess the quantities of detergent bound to purified MPs, thus enabling the quantification of close structure detergents via a single procedure. This HPTLC method, which is fast and requires low sample volume, is fully suitable for routine measurements. Copyright © 2013 Elsevier B.V. All rights reserved.

  4. Quantitative determination of seven chemical constituents and chemo-type differentiation of chamomiles using high-performance thin-layer chromatography

    Science.gov (United States)

    Matricaria recutita L. (German Chamomile), Anthemis nobilis L. (Roman Chamomile) and Chrysanthemum morifolium Ramat are commonly used chamomiles. High performance thin layer chromatographic (HPTLC) method was developed for estimation of six flavonoids (rutin, luteolin-7-O-ß-glucoside, chamaemeloside...

  5. Thin-layer chromatography method for the simultaneous quantification and stability testing of alprazolam and mebeverine in their combined pharmaceutical dosage form

    National Research Council Canada - National Science Library

    Chhalotiya, Usmangani K; Patel, Nishma M; Shah, Dimal A; Mehta, Falgun A; Bhatt, Kashyap K

    2017-01-01

    A sensitive, selective and precise high-performance thin-layer chromatographic method was developed and validated for the simultaneous determination of alprazolam and mebeverine, both as bulk drugs and in formulations...

  6. Forensic examination of ink by high-performance thin layer chromatography--the United States Secret Service Digital Ink Library.

    Science.gov (United States)

    Neumann, Cedric; Ramotowski, Robert; Genessay, Thibault

    2011-05-13

    Forensic examinations of ink have been performed since the beginning of the 20th century. Since the 1960s, the International Ink Library, maintained by the United States Secret Service, has supported those analyses. Until 2009, the search and identification of inks were essentially performed manually. This paper describes the results of a project designed to improve ink samples' analytical and search processes. The project focused on the development of improved standardization procedures to ensure the best possible reproducibility between analyses run on different HPTLC plates. The successful implementation of this new calibration method enabled the development of mathematical algorithms and of a software package to complement the existing ink library. Copyright © 2010 Elsevier B.V. All rights reserved.

  7. A Hyphenated Technique based on High-Performance Thin Layer Chromatography for Determining Neutral Sphingolipids: A Proof of Concept

    Directory of Open Access Journals (Sweden)

    Andrés Domínguez

    2015-04-01

    Full Text Available Hyphenated HPTLC has been used to analyze several neutral sphingolipids acting as lysosomal storage disease (LSD biomarkers. Automated multiple development (AMD provides separation of lipid peaks, which are detected and quantified using fluorescence detection by intensity changes (FDIC after primuline post-impregnation. A final online transfer to a mass spectrometer by means of an elution-based interface allows their identification using electrospray ionization (ESI and atmospheric pressure chemical ionization (APCI.Given that the increases in fluorescent emission detected by FDIC are produced by non-specific, electrostatic interactions between the primuline and hydrocarbon chains in the ceramide backbones of sphingolipids, it is a non-destructive detection technique, allowing the precise location and transfer of biomarker peaks to a mass spectrometer using an elution interface. By using primuline as a fluorophore, the technique is also compatible with ESI-APCI and does not interfere with the MS of sphingolipids. APCI provides useful and complementary structural information to the ESI for sphingolipid identification. Moreover, FDIC emission can be used for quantitative purposes. Results include the determination of sphingomyelin (SM in human-plasma samples (RSD < 6% by means of a standard addition method with non-linear calibration, and the identification of globotriaosylceramide (Gb3 in the plasma of a Fabry patient. Only one HPTLC plate is needed to perform the analysis.

  8. Densitometric Validation and Optimisation of Polyphenols in Ocimum sanctum Linn by High Performance Thin-layer Chromatography.

    Science.gov (United States)

    U K, Ilyas; Katare, Deepshikha P; Aeri, Vidhu

    2015-01-01

    Ocimum sanctum Linn (Sanskrit: Tulasi; family: Libiaceae), popularly known as holy basil or Ocimum teinufolium, is found throughout the semitropical and tropical parts of India. In Ayurveda, Tulasi has been well known for its therapeutic potentials. To optimise and develop a standard method to quantify seven polyphenols simultaneously by HPTLC. A three-level factor Box-Behnken statistical design was used for optimisation, where extraction time (min), temperature (°C) and methanol:water ratio (% v/v) are the independent variables with polyphenols as the dependent variable. The separation was archived on a silica-gel 60 F254 HPTLC plate using toluene:ethyl acetate:formic acid:methanol (3:3:0.8:0.2 v/v) as the mobile phase. Densitometric analysis of polyphenols was carried out in the absorbance mode at 366 nm. The quantification of polyphenols was carried out based on peak area with a linear calibration curve at concentration ranges of 60-240, 20-200, 100-1600, 40-200, 200-1400, 10-160, 200-1400, 100-5000 ng/band for caffeic acid, ellagic acid, rutin, kaempferol, catechin, quercetin, eupalitin and epicatechin respectively. The method was validated for peak purity, precision, accuracy, limit of detection (LOD) and quantification (LOQ). Method specificity was confirmed using the retention factor value and visible spectra correlation of marker compounds. A validated HPTLC method was newly developed for simultaneous quantification of seven polyphenols in an Ayurvedic preparation of O. sanctum. The proposed method is simple, precise, specific, accurate, cost-effective, less time consuming and has the ability to separate the polyphenols from other constituents. Copyright © 2015 John Wiley & Sons, Ltd.

  9. Suitability of thin-layer chromatography-flame ionization detection with regard to quantitative characterization of different fossil fuel products. II. Calibration methods concerning quantitative hydrocarbon-group type analysis

    Energy Technology Data Exchange (ETDEWEB)

    Vela, J.; Membrado, L.; Cebolla, V.L.; Ferrando, A.C. [CSIC, Zaragoza (Spain). Inst. de Carboquimica, Dept. de Procesos Quimicos

    1998-10-01

    Time-consuming external standard-based calibration methods are usually performed for hydrocarbon group type analysis (HGTA) of fossil fuels, regardless of the instrumental chromatographic technique. HGTA of a broad variety of coal and petroleum products was performed using a modern thin-layer chromatography-flame ionization detection (TLC-FID) system and a rapid method based on internal normalization. Repeatability, linear intervals, and sample load ranges for quantitative application of this method are given, namely a heavy oil and its derived hydrocracked products, raw and chemically-modified petroleum asphaltenes, a coal-tar pitch, several coal extracts, and coal hydroliquefaction products. Results from external standard calibration and a normalization method (both obtained by TLC-FID) are in agreement, and they are validated using TLC-ultraviolet scanning. The use of the latter demonstrates that TLC-FID can also be applied to products such as coal extracts and hydroliquefaction products, despite these products being more volatile than petroleum asphaltenes or heavy oils. 14 refs., 3 figs., 5 tabs.

  10. A thin-layer chromatography method for the identification of three different olibanum resins (Boswellia serrata, Boswellia papyrifera and Boswellia carterii, respectively, Boswellia sacra).

    Science.gov (United States)

    Paul, Michael; Brüning, Gerit; Bergmann, Jochen; Jauch, Johann

    2012-01-01

    Resins of the genus Boswellia are currently an interesting topic for pharmaceutical research since several pharmacological activities (e.g. anti-inflammatory, anti-microbial, anti-tumour) are reported for extracts and compounds isolated from them. Unambiguous identification of these resins, by simple and convenient analytical methods, has so far not clearly been verified. For differentiation and identification of three important Boswellia species (Boswellia serrata Roxb., Boswellia papyrifera Hochst. and Boswellia carterii Birdw., respectively Boswellia sacra Flueck.), possible even for minimally equipped laboratories, a thin-layer chromatography (TLC) method was developed, allowing unambiguous identification of the three species. Crude resin samples (commercial samples and a voucher specimen) were extracted with methanol or diethyl ether and subjected to TLC analysis (normal phase). A pentane and diethyl ether (2:1) with 1% acetic acid eluent was used. Chromatograms were analysed by UV detection (254 nm) and dyeing with anisaldehyde dyeing reagent. Significant spots were isolated and structures were assigned (mass spectrometry; nuclear magnetic resonance spectroscopy). Incensole and incensole acetate are specific biomarkers for Boswellia papyrifera. Boswellia carterii/Boswellia sacra reveal ß-caryophyllene oxide as a significant marker compound. Boswellia serrata shows neither incensole acetate nor ß-caryophyllene oxide spots, but can be identified by a strong serratol and a sharp 3-oxo-8,24-dien-tirucallic acid spot. The TLC method developed allows unambiguous identification of three different olibanum samples (Boswellia papyrifera, Boswellia serrata, Boswellia carterii/Boswellia sacra). Evidence on the specific biosynthesis routes of these Boswellia species is reported. Copyright © 2011 John Wiley & Sons, Ltd.

  11. Determinação de aflatoxina B1 em pimenta (Piper nigrum L. e orégano (Origanum vulgare L. por cromatografia em camada delgada e densitometria Determination of aflatoxin B1 (Piper nigrum L. and oregano (Origanum vulgare L. by thin-layer chromatography and densitometry

    Directory of Open Access Journals (Sweden)

    Guilherme Prado

    2008-01-01

    Full Text Available An analytical study based on extraction with methanol-water, immunoaffinity cleanup and separation, identification and quantification of aflatoxin B1 by thin-layer chromatography,in ground black and white pepper and oregano was carried out. Validation of the applied methodology was done through accuracy and precision studies. Recoveries of aflatoxin B1 and relative standard deviations, from spice samples spiked at levels from 4.86 to 97.70 µg/kg, were, respectively, higher than 72% and lower than 20%. Application to spice samples available in Minas Gerais state, purchased at popular markets, showed no contamination with aflatoxin B1.

  12. Plant-determined variation in cardenolide content and thin-layer chromatography profiles of monarch butterflies,Danaus plexippus reared on milkweed plants in California : 3. Asclepias californica.

    Science.gov (United States)

    Brower, L P; Seiber, J N; Nelson, C J; Lynch, S P; Hoggard, M P; Cohen, J A

    1984-12-01

    Variation in gross cardenolide concentration of the mature leaves of 85Asclepias californica plants collected in four different areas of California is a positively skewed distribution ranging from 9 to 199 μg of cardenolide per 0.1 g dry weight with a mean of 66 μg/0.1 g. Butterflies reared individually on these plants in their native habitats contained a normal distribution of cardenolide ranging from 59 to 410 μg of cardenolide per 0.1 g dry weight with a mean of 234 μg. Cardenolide uptake by the butterflies was a logarithmic function of plant concentration. Total cardenolide per butterfly ranged from 143 to 823 μg with a mean of 441 μg and also was normally distributed. Populational variation of plant cardenolide concentrations occurs within subspecies, but the northern subspeciesA. c. greenei does not differ significantly from the southernA. c. californica. Generally higher concentrations occur in butterflies from northern populations and in females. No evidence was adduced that cardenolides in the plants adversely affected the butterflies. Low cardenolide concentrations in the leaves and the absence of cardenolides in the latex characterize bothA. californica andA. speciosa, but notA. eriocarpa. Thin-layer chromatography in two solvent systems isolated 24 cardenolide spots in the plants, of which 18 are stored by the butterflies. There was a minor difference in the cardenolide spot patterns due to geographic origin of the plants, but as in our previous studies, none in the sexes of the butterflies. UnlikeA. eriocarpa andA. speciosa, A. californica plants lack cardenolides withRf values greater than digitoxigenin. Overall, the cardenolides of bothA. californica andA. speciosa are more polar than those inA. eriocarpa. A. californica plants contain cardenolides of the calotropagenin series including calotropin, calactin, and uscharidin, and the latter is metabolically transformed by monarch larvae to calactin and calotropin. Cardenolides of this series also

  13. Linear modeling of the soil-water partition coefficient normalized to organic carbon content by reversed-phase thin-layer chromatography.

    Science.gov (United States)

    Andrić, Filip; Šegan, Sandra; Dramićanin, Aleksandra; Majstorović, Helena; Milojković-Opsenica, Dušanka

    2016-08-05

    Soil-water partition coefficient normalized to the organic carbon content (KOC) is one of the crucial properties influencing the fate of organic compounds in the environment. Chromatographic methods are well established alternative for direct sorption techniques used for KOC determination. The present work proposes reversed-phase thin-layer chromatography (RP-TLC) as a simpler, yet equally accurate method as officially recommended HPLC technique. Several TLC systems were studied including octadecyl-(RP18) and cyano-(CN) modified silica layers in combination with methanol-water and acetonitrile-water mixtures as mobile phases. In total 50 compounds of different molecular shape, size, and various ability to establish specific interactions were selected (phenols, beznodiazepines, triazine herbicides, and polyaromatic hydrocarbons). Calibration set of 29 compounds with known logKOC values determined by sorption experiments was used to build simple univariate calibrations, Principal Component Regression (PCR) and Partial Least Squares (PLS) models between logKOC and TLC retention parameters. Models exhibit good statistical performance, indicating that CN-layers contribute better to logKOC modeling than RP18-silica. The most promising TLC methods, officially recommended HPLC method, and four in silico estimation approaches have been compared by non-parametric Sum of Ranking Differences approach (SRD). The best estimations of logKOC values were achieved by simple univariate calibration of TLC retention data involving CN-silica layers and moderate content of methanol (40-50%v/v). They were ranked far well compared to the officially recommended HPLC method which was ranked in the middle. The worst estimates have been obtained from in silico computations based on octanol-water partition coefficient. Linear Solvation Energy Relationship study revealed that increased polarity of CN-layers over RP18 in combination with methanol-water mixtures is the key to better modeling of

  14. Analysis of α-mangostin in the herbal drinks of mangosteen rind (Garcinia mangostana L. by thin layer chromatography-densitometric method

    Directory of Open Access Journals (Sweden)

    Regina Andayani

    2017-12-01

    Full Text Available Some herbal formulation containing α-mangostin as a marker compound in the pericarp of the mangosteen (Garcinia mangostana L. are marketed now in Indonesia. The determination of the component of preparation both qualitatively and quantitatively is essential to ensure quality of the product. This research is aimed to develop a TLC (Thin Layer Chromatography-densitometry method to analyze α-mangostin in the herbal drinks of mangosteen rind. The analysis was performed with TLC Scanner using Camag TLC Scanner 4 with Wincats software. Silica gel 60 F254 (Merck plates (20x20 cm: 200 μm thickness were used as stationary phase and mixture of chloroform and ethyl acetate (9:1,v/v as a mobile phase. The developed chromatogram was scanned at 316 nm, the wavelength of maximum absorption for α-mangostin. At this condition, the Rf value of α-mangostin is 0.48. Regression analysis of the calibration data showed an excellent linear relationship between peak-area vs drug concentration. Linearity was found to be in the range of 50-400 µg/mL. The suitability of developed TLC densitometry method for estimation of α-mangostin was established by validating it as per the ICH guidelines. The limits of detection (LOD and quantification (LOQ for α-mangostin were found to be 54.38 μg/mL and 181.28 μg/mL. The developed method was found to be linear (r=0,99415, precise (RSD <1.28 % and < 2.39 % for intra-day and inter-day precision and accurate (mean recovery of 90.04%. Results of the samples analysis showed that sample A does not contain α-mangostin, whereas sample B and C contain α-mangostin. The average concentrations obtained for samples B and C were 0.040% w/v and 0.118% w/v, respectively. The developed method has been successfully applied for the determination of α-mangostin in the herbal drinks of mangosteen rind.

  15. Assay for trenbolone and its metabolite 17 alpha-trenbolone in bovine urine based on immunoaffinity chromatographic clean-up and off-line high-performance liquid chromatography-thin-layer chromatography.

    Science.gov (United States)

    van Ginkel, L A; van Blitterswijk, H; Zoontjes, P W; van den Bosch, D; Stephany, R W

    1988-07-22

    An high-performance liquid chromatography (HPLC)-thin-layer chromatography (TLC) method was developed to detect the illegal use of the xenobiotic growth promotor Trenbolone acetate (TBA). Very effective clean-up of bovine urine was achieved by immunoaffinity chromatography (IAC). The active form of TBA, the steroid 17 beta-Trenbolone (17 beta-TB), as well as its major metabolite 17 alpha-Trenbolone (17 alpha-TB), were assayed simultaneously with HPLC and on-line UV detection. The fraction containing 17 alpha-TB and 17 beta-TB (TB-fraction) was collected, and for confirmation 17 beta- and 17 alpha-TB were subsequently separated and identified by TLC. The limit of detection by on-line HPLC-UV (350 nm) was 1-2 micrograms TB/l. Off-line TLC detection was even more sensitive, 0.5 microgram 17 beta- or 17 alpha-TB/1. The assay was validated by investigating urine samples from veal calves implanted with TBA. The presence of 17 beta- and 17 alpha-TB was clearly demonstrated. A survey of the illegal use of TBA in cattle was performed by applying the assay to urine obtained at slaughter. No residues of TBA or its metabolites were found in any of the 144 random samples from the Dutch public health surveillance programme.

  16. High performance thin layer chromatography (HPTLC) and high performance liquid chromatography (HPLC) for the qualitative and quantitative analysis of Calendula officinalis-advantages and limitations.

    Science.gov (United States)

    Loescher, Christine M; Morton, David W; Razic, Slavica; Agatonovic-Kustrin, Snezana

    2014-09-01

    Chromatography techniques such as HPTLC and HPLC are commonly used to produce a chemical fingerprint of a plant to allow identification and quantify the main constituents within the plant. The aims of this study were to compare HPTLC and HPLC, for qualitative and quantitative analysis of the major constituents of Calendula officinalis and to investigate the effect of different extraction techniques on the C. officinalis extract composition from different parts of the plant. The results found HPTLC to be effective for qualitative analysis, however, HPLC was found to be more accurate for quantitative analysis. A combination of the two methods may be useful in a quality control setting as it would allow rapid qualitative analysis of herbal material while maintaining accurate quantification of extract composition. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. ⁶⁸Ge content quality control of ⁶⁸Ge/⁶⁸Ga-generator eluates and ⁶⁸Ga radiopharmaceuticals--a protocol for determining the ⁶⁸Ge content using thin-layer chromatography.

    Science.gov (United States)

    Eppard, Elisabeth; Loktionova, Natalia S; Rösch, Frank

    2014-09-01

    (68)Ge breakthrough from a (68)Ge/(68)Ga-generator appears to be one of the most critical parameters for the routine clinical application of this generator and (68)Ga-radiopharmaceuticals. We report a TLC-based (thin-layer chromatography) protocol which allows the (68)Ge breakthrough of a generator to be determined within 1 h post-initial elution. The protocol can also be adapted to allow the (68)Ge content of a (68)Ga-radiopharmaceutical preparation to be determined prior to in vivo application. Copyright © 2014 Elsevier Ltd. All rights reserved.

  18. Analytical strategy for rapid identification and quantification of lubricant additives in mineral oil by high-performance thin-layer chromatography with UV absorption and fluorescence detection combined with mass spectrometry and infrared spectroscopy.

    Science.gov (United States)

    Dytkiewitz, Elisabeth; Morlock, Gertrud E

    2008-01-01

    A simple strategy for identification and quantification of lubricant additives in mineral oil was demonstrated by high-performance thin-layer chromatography with UV absorption and fluorescence detection using various coupling options, e.g., with attenuated total reflectance infrared (ATR-IR) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, electrospray ionization mass spectrometry (ESI-MS), and direct analysis in real-time mass spectrometry (DART-MS). For the additives zinc bis(O,O'-diisobutyl dithiophosphate), zinc bis(O,O'-didodecyl dithiophosphate), and Anglamol 99, 2 chromatographic systems were developed, i.e., a reversed-phase (RP) system on RP2 plates using an acetonitrile-based mobile phase and a normal-phase system on silica gel 60 plates using a toluene-based gradient. Densitometry was performed by absorption measurement at 220 nm. Repeatabilities (relative standard deviation, n = 6) between 2.2 and 5.5% and correlation coefficients >0.9973 were highly satisfactory for the analysis of these additives in the mineral oil. Primuline reagent was used to improve the detection limit of the lipophilic additives by a factor of 2, followed by fluorescence measurement at UV 366/>400 nm. For rapid identification by ATR-IR and FTIR, the respective additive zones on the plate were online extracted by an interface called ChromeXtract, concentrated, and directly applied for measurements in the wave number range of 4000-400 cm(-1). Identification was confirmed by online ESI-MS within a minute using ChromeXtract and by DART-MS within seconds.

  19. Thin-layer chromatography method for the simultaneous quantification and stability testing of alprazolam and mebeverine in their combined pharmaceutical dosage form

    OpenAIRE

    Chhalotiya, Usmangani K.; Patel, Nishma M.; SHAH, Dimal A.; Mehta, Falgun A.; Bhatt, Kashyap K.

    2017-01-01

    A sensitive, selective and precise high-performance thin-layer chromatographic method was developed and validated for the simultaneous determination of alprazolam and mebeverine, both as bulk drugs and in formulations. The method employed HPTLC aluminium plates that had been pre-coated with silica gel 60F-254 as the stationary phase, while the solvent system was acetone:methanol:acetic acid (6:4:0.1, v/v/v). The Rf values of alprazolam and mebeverine were observed to be 0.80 ± 0.08 and 0.60 ±...

  20. Phytochemical screening and thin layer chromatographic profile of ...

    African Journals Online (AJOL)

    The present study investigates the phytochemicals and thin layer chromatographic profile of. Nauclea diderrichii (Rubiaceae) leaf extracts. Phytochemical in the hexane, ethyl acetate and methanol extracts were determined using standard chemical tests. Thin layer chromatographic techniques were carried out using various ...

  1. Detection of the potential adulterant Teucrium chamaedrys in Scutellaria baicalensis raw material and extract by high-performance thin-layer chromatography.

    Science.gov (United States)

    Hong, Thao; Jeong, Mijeong Lee; Zahn, Michael; Fay, Brooke A; Lee, Kangwoo; Hwangbo, Huunjung; Park, Eunhye; Kim, Minjung; Ma, Wenwen

    2009-01-01

    Teucrium chamaedrys (Gemander) has been reported as an adulterant of Scutellaria lateriflora (American skullcap) herbal preparations and is also known to be hepatotoxic. A quick and simple high-performance thin-layer chromatographic (HPTLC) method was developed for the detection of T. chamaedrys (Germander) in S. baicalensis (Chinese skullcap) extract, an ingredient of the proprietary blend product, Univestin. The HPTLC profile of T. chamaedrys was distinguished from that of S. baicalensis by its bright green fluorescence bands. This simple method can be completed in an hour for the quality control of Univestin and its raw material, S. baicalensis. The method is sensitive and can detect T. chamaedrys at levels as low as 0.5% (w/w).

  2. Patch testing with thin-layer chromatograms of chamomile tea in patients allergic to sesquiterpene lactones.

    Science.gov (United States)

    Lundh, Kerstin; Gruvberger, Birgitta; Möller, Halvor; Persson, Lena; Hindsén, Monica; Zimerson, Erik; Svensson, Ake; Bruze, Magnus

    2007-10-01

    Patients with contact allergy to sesquiterpene lactones (SLs) are usually hypersensitive to Asteraceae plant products such as herbal teas. The objective of this study was to show sensitizers in chamomile tea by patch testing with thin-layer chromatograms. Tea made from German chamomile was separated by thin-layer chromatography. Strips of the thin-layer chromatograms were used for patch testing SL-positive patients. 15 (43%) of 35 patients tested positively to 1 or more spots on the thin-layer chromatogram, with many individual reaction patterns. Patch testing with thin-layer chromatograms of German chamomile tea showed the presence of several allergens.

  3. A validated high-performance thin-layer chromatography method for the identification and simultaneous quantification of six markers from Platanus orientalis and their cytotoxic profiles against skin cancer cell lines.

    Science.gov (United States)

    Khan, Imran; Sangwan, Payare L; Dar, Alamgir A; Rafiq, Rather A; Farrukh, Mufti R; Dhar, Jagdish K; Tasduq, Sheikh A; Koul, Surrinder

    2013-08-01

    Betulinic acid (1), betulinic acid-3-acetate (2), 3-acetylbetulinaldehyde (3), oleanolic acid-3-acetate (4), 3-β-hydroxy-28,19-β-olenolide (5), and β-sitosterol (6) were isolated from Platanus orientalis and a high-performance thin-layer chromatography method was developed for their simultaneous quantification. The markers were first derivatized on the chromatogram with ceric ammonium sulfate and then high-performance thin-layer chromatography densitometry was carried out. Chromatographic separation of these markers was carried out on silica gel 60 plates using a ternary solvent system n-hexane/toluene/acetone (6:3.5:1 v/v/v) as a mobile phase. For marker 1, a deuterium (D2) lamp and wavelength of 420 nm was used. A tungsten (W) lamp was used for markers 2 and 3 at 550 nm and for 4-6 at 500 nm. The method was validated for accuracy, precision, LOD, and LOQ. All calibration curves showed a good linear relationship (r > 0.9919). The precision evaluated by an intra- and interday study showed RSDs < 2.51% and accuracy validation recovery between 95.54 and 99.33% with RSDs < 1.55%. The successful application of the validated method showed 1 as the most abundant component (4.63%) and 5 (0.017%) the least. The markers displayed a significant cytotoxic effect against human keratinocyte, mouse melanoma, and human skin epithelial carcinoma cancer cells by using a 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Using of scanner on the evaluation of pesticides mobility by thin-layer chromatography; Utilizacao do scanner na avaliacao da mobilidade de agrotoxicos por cromatografia de camada delgada

    Energy Technology Data Exchange (ETDEWEB)

    Tornisielo, V.L.; Costa, M.A.; Furlan, G.R. [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil)

    1995-12-31

    Knowledge of pesticide leaching potential is an essential information to preview environmental fate. The experiment confirms the possibility of using radiochromatogram scanning as a substitute for X-ray autoradiography, when Thin Layer Chromatografy (TLC) methodogy is used to determine mobility of a pesticide. Three types of soil from Sao Paulo state and five herbicides (metolachlor, asulan, simazing, 2,4-D and trifluralin), labeled with {sup 14} C, were used. The radiochromatogram scanners permits a quick detection of the position of the radioactive spots to determine the Rf for each pesticide, while X-ray film has to be placed on the plate on the dark room for several days or weeks and then developed to detect spots, subsequently measure and calculate Rf. The results showed that the evaluation by scanner and X-ray were similar. Hence we conclude that the use of the scanner should be considered since this methodology is faster and as accurate as the X-ray methodology. (author). 4 refs, 1 fig, 2 tabs.

  5. Determination of alpha-solanine and alpha-chaconine in potatoes by high-performance thin-layer chromatography/densitometry.

    Science.gov (United States)

    Bodart, P; Kabengera, C; Noirfalise, A; Hubert, P; Angenot, L

    2000-01-01

    A high-performance thin-layer chromatographic (HPTLC) method was used to determine the glycoalkaloids alpha-solanine and alpha-chaconine in potatoes. Alpha-solanine and alpha-chaconine are extracted from dehydrated potatoes with boiling methanol-acetic acid (95 + 5, v/v). The analytes are separated on a Silica Gel 60 F254 HPTLC plate by a saturated mixture of dichloromethane-methanol-water-concentrated ammonium hydroxide (70 + 30 + 4 + 0.4, v/v), which is used for vertical development of the plate up to a distance of 85 mm. For visualization, the plate is dipped 3 times into a modified Carr-Price reagent, 20% (w/v) antimony(III) chloride in acetic acid-dichloromethane (1 + 3, v/v), and subsequently heated on a hot plate at 105 degrees C for 5 min. The glycoalkaloids all appear as red chromatographic zones on a colorless background. Densitometric quantification is performed at 507 nm by reflectance scanning. After determination of the appropriate response function, the proposed method was validated. Good results with respect to linearity, accuracy, and precision were obtained in the concentration range studied.

  6. Analysis of native milk oligosaccharides directly from thin-layer chromatography plates by matrix-assisted laser desorption/ionization orthogonal-time-of-flight mass spectrometry with a glycerol matrix.

    Science.gov (United States)

    Dreisewerd, Klaus; Kölbl, Stefanie; Peter-Katalinić, Jasna; Berkenkamp, Stefan; Pohlentz, Gottfried

    2006-02-01

    We have recently presented a new method for direct coupling of high-performance thin-layer chromatography (HPTLC) with matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS), illustrated by the analysis of a complex ganglioside mixture. In the current communication, an adaptation of this procedure to mixtures of native oligosaccharides from human and from elephant milk is described. The key features in this method are (1) glycerol as a liquid matrix, to provide a homogeneous wetting of the silica gel and a simple and fast MALDI preparation protocol, (2) an infrared (IR) laser for volume material ablation and particular soft desorption/ionization conditions, and (3) an orthogonal time-of-flight mass spectrometer for a high mass accuracy, independent of any irregularity of the silica gel surface. Chromatographic "mobility profiles" were determined by scanning the laser beam across the analyte bands. The current limit of detection for the MS analysis was determined to approximately 10 pmol of individual oligosaccharides spotted for chromatography. A liquid composite matrix, containing glycerol and the ultraviolet (UV-)MALDI matrix alpha-cyano-4-hydroxycinnamic acid, allows a direct HPTLC-MALDI-MS analysis with a 337 nm-UV laser as well. Compared to the IR-MALDI mode, the analytical sensitivity in UV-MALDI was found to be lower by one order of magnitude, whereas unspecific analyte ion fragmentation as well as adduct formation was found to be more extensive.

  7. Comparison of two detection methods in thin layer chromatographic ...

    African Journals Online (AJOL)

    o-tolidine plus potassium iodide and photosynthesis inhibition detection methods were investigated for the analysis of three triazine herbicides (atrazine, ametryne, simazine) and two urea herbicides (diuron, metobromuron) in a coastal savanna soil using thin layer chromatography to compare the suitability of the two ...

  8. Comparison of Two Detection Methods in Thin Layer ...

    African Journals Online (AJOL)

    komla

    Abstract o-tolidine plus potassium iodide and photosynthesis inhibition detection methods were investigated for the analysis of three triazine herbicides (atrazine, ametryne, simazine) and two urea herbicides (diuron, metobromuron) in a coastal savanna soil using thin layer chromatography to compare the suitability of the ...

  9. Direct extraction of urinary analytes from undeveloped reversed-phase thin layer chromatography plates using a solvent gradient combined with on-line electrospray ionisation ion mobility-mass spectrometry.

    Science.gov (United States)

    Devenport, Neil A; Reynolds, James C; Weston, Daniel J; Wilson, Ian D; Creaser, Colin S

    2012-08-07

    The direct extraction of urinary analytes deposited on reversed-phase thin-layer chromatography (RP-TLC) plates is demonstrated using a solvent gradient extraction procedure without prior chromatographic development. The surface sample probe TLC-MS interface used for the gradient extraction is compared to direct loop injection into the electrospray ion source for biofluid profiling. The gradient elution is shown to enhance ion intensities, as urinary salts are eluted in aqueous formic acid in the early part of the gradient reducing ion suppression. The retention of urinary components on the C18 RP-TLC plate was confirmed by monitoring analyte responses with, and without, an aqueous wash phase prior to the solvent gradient extraction. The use of gradient elution allows fractionation of the complex biological matrix as a result of differential retention of urine components on the undeveloped RP-TLC plate. The direct gradient analysis of TLC plates has also been combined with ion mobility-mass spectrometry to further resolve the complex urinary profile and identify co-eluting compounds.

  10. Cromatografia em camada delgada para o diagnóstico da intoxicação por aldicarb ("chumbinho" em cães e gatos Thin-layer chromatography for aldicarb poisoning diagnosis in dogs and cats

    Directory of Open Access Journals (Sweden)

    F.G. Xavier

    2007-10-01

    Full Text Available Avaliou-se a cromatografia em camada delgada (CCD como método de diagnóstico toxicológico para os casos de intoxicação por aldicarb em cães e gatos, utilizando-se 50 amostras de conteúdo gástrico obtidas durante a necropsia e 50 amostras de alimentos utilizados como iscas para intoxicar criminalmente os animais. Todas as amostras resultaram positivas para o aldicarb, mostrando ser a CCD uma técnica qualitativa eficiente, rápida e de baixo custo, com uso potencial na toxicologia veterinária forense.The present study concerns about the identification of aldicarb residues using thin-layer chromatography (TLC in 50 samples of gastric content obtained from the necropsy of dogs and cats and 50 samples of foods suspected of being used as baits. All samples resulted positive for aldicarb showing that the TLC is an efficient, fast and not expensive qualitative method for the detection of aldicarb, being useful for this purpose in the forensic veterinary toxicology.

  11. Physicochemical properties of silica gel coated with a thin layer of polyaniline (PANI) and its application in non-suppressed ion chromatography.

    Science.gov (United States)

    Sowa, Ireneusz; Kocjan, Ryszard; Wójciak-Kosior, Magdalena; Swieboda, Ryszard; Zajdel, Dominika; Hajnos, Mieczysław

    2013-10-15

    Physicochemical properties of a new sorbent and its potential application in non-suppressed ion chromatography (IC) have been investigated. The sorbent was obtained in a process of covering silica gel particles with a film of polyaniline (PANI). The properties of silica modified with polyaniline such as particle size, porosity, average quantity of polyaniline covering carrier and density of sorbent were determined. In our study the following methods were used: microscopic analysis, laser diffraction technique, combustion analysis, mercury porosimetry and helium pycnometry. Column with the newly obtained packing was used for the separation of inorganic anions. Optimized chromatographic system was successfully employed for analysis of iodide and bromide in selected pharmaceutical products (Bochnia salt and Iwonicz salt) applied in chronic respiratory disease. Analysis was carried out using 0.1M solution of HCl in mixture of methanol/water (50:50v/v) as a mobile phase; the flow rate was 0.3 mL min(-1), temperature was 24°C and λ=210 nm. Validation parameters such as correlation coefficient, RSD values, recovery, detection and quantification limits were found to be satisfactory. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. High-performance thin-layer chromatography based concurrent estimation of biomarkers ent-phyllanthidine and rutin in the dried aerial parts of Flueggea virosa

    Directory of Open Access Journals (Sweden)

    Nasir A. Siddiqui

    2017-07-01

    Full Text Available The biomarkers are needed to be defined for standardization purposes so that safe and effective herbal formulations can be catered to the society. There is an urgent need for statistical support of herbal drugs because most of the herbal products are still used in the non-standardized form. This study is based on the development of a simple and sensitive RP-HPTLC method for concurrent estimation of two biomarkers ent-phyllanthidine and rutin in the methanol extract of aerial parts of Flueggea virosa. The developed method was found to be simple, economic and sensitive. Separation and quantification were performed with acetonitrile: water (4:6 V/V used as the mobile phase on glass-backed RP-HPTLC plate. Detection of absorption maxima and quantification was done at 310 nm of UV region. The developed chromatographic system was found to give a sharp band for ent-phyllanthidine and rutin at Rf 0.73 ± 0.01 and 0.68 ± 0.01, respectively. The linearity ranges for ent-phyllanthidine, and rutin were found to be 200–1600 ngband−1 and 100–1400 ngband−1, respectively, with correlation coefficients (r2 values of 0.998 and 0.997, respectively. The percentage of ent-phyllanthidine and rutin was found to be 9.121 ± 0.02% and 1.018 ± 0.04% (w/w, respectively. The resolution of bands and separation of constituents in FVME exhibited the perfect optimization of the developed method. The validation statistics supports the proposed method for standardizing crude drugs as well as formulations of a natural product containing ent-phyllanthidine and rutin.

  13. Validation of the FDG (18F) radiochemical purity assay by thin layer chromatography; Validacao do ensaio de pureza radioquimica do FDG (18F) por cromatografia em camada delgada

    Energy Technology Data Exchange (ETDEWEB)

    Leao, R.L.C.; Oliveira, M.L.; Nascimento, J.E.; Nascimento, N.C.E.S., E-mail: renata.lleao@hotmail.com [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil). Div. de Producao de Radiofarmacos

    2013-08-15

    All methodologies utilized in radiopharmaceutical industry should be validated in order to prove that they meet the requirements of analytical applications, ensuring the reliability of the results. At a radiopharmaceutical industry there is one challenge aspect: sometimes it is not possible use a stable standard to perform the validation analysis. In order to overcome this difficulty, the objective of this study was to suggest a validation protocol for these methodologies, based on the recommendations of RE n° 899/Agencia Nacional de Vigilancia Sanitaria (ANVISA), and prove its efficiency, performing the radiochemical purity validation test of FDG (18F), by TLC. To obtain the calibration curve, we suggested that the theoretical activity values should be determined using a dose calibrator, simultaneously of each analysis performed by TLC, for 5 hours. The method was linear (R{sup 2} of 0.996), precise (CV% <5%) and accurate (96.85% < accuracy < 102.56%). In relation to the robustness test, our experiments evaluated the influence of the distance travelled by mobile phase, variations at mobile phase concentration and type of chromatographic plate (silica gel on glass or aluminium plates). The detection and quantification limits were determined (321.9 and 1065.6 kBq, respectively). As expected, this methodology was nonspecific, showing a slight spot corresponding to the FDM. The proposed protocol was efficient and the methodology tested was effective to determine the radiochemical purity of FDG (18F), in accordance to the limits recommended by ANVISA. (author)

  14. Correct assignment of lipophilic dye mixtures? A case study for high-performance thin-layer chromatography-mass spectrometry and performance data for the TLC-MS Interface.

    Science.gov (United States)

    Morlock, Gertrud E; Brett, Neil

    2015-04-17

    The TLC-MS Interface, the successor of the ChromeXtract, has been available for elution head-based coupling of high-performance thin-layer chromatography with mass spectrometry (HPTLC-MS) since 2009, and is meanwhile widespread in use, mainly for compound confirmation. Until now, quantitative performance data has not been reported in detail and thus were investigated in this study. The performance data of HPTLC-electrospray ionization (ESI)-MS via the TLC-MS Interface showed good mean precisions (%RSD, n=5) for 6 dyes in a commercially available dye mixture investigated at two different concentrations (7.3% for the 1:8 dilution, and 10.1% for the 1:16 diluted) in a selected worst case scenario. The respective mean precisions of absorbance measurements were ≤1.3%. For calibrations by HPTLC-ESI-MS, the mean determination coefficient was 0.9975 for the 6 dyes (versus 0.9997 for absorbance measurement). HPTLC-MS analysis revealed the incorrect assignment of components in two commercially available dye mixtures. Using an additional software (MassWorks) that delivered a 100 times increased mass accuracy, the proposal of molecular formulae was shown to be obtainable under certain conditions with a low resolution single quadrupole mass spectrometer and in the case of helpful information such as the double bond equivalents. This enabled the identification of the incorrectly assigned unknown dyes and clearly demonstrated the benefit of using HPTLC-MS for zone confirmation. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Analysis of gangliosides directly from thin-layer chromatography plates by infrared matrix-assisted laser desorption/ionization orthogonal time-of-flight mass spectrometry with a glycerol matrix.

    Science.gov (United States)

    Dreisewerd, Klaus; Müthing, Johannes; Rohlfing, Andreas; Meisen, Iris; Vukelić, Zeljka; Peter-Katalinić, Jasna; Hillenkamp, Franz; Berkenkamp, Stefan

    2005-07-01

    A novel method is presented for direct coupling of high-performance thin-layer chromatography (HPTLC) with matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) for the analysis of biomolecules. A first key feature is the use of a liquid matrix (glycerol), which provides a homogeneous wetting of the silica gel and a simple and fast MALDI preparation protocol. A second is the use of an Er:YAG infrared laser, which ablates layers of approximately 10-microm thickness of analyte-loaded silica gel and provides a soft desorption/ionization of even very labile analyte molecules. The orthogonal time-of-flight mass spectrometer employed in this study, finally provides a high accuracy of the mass determination, which is independent of any irregularity of the silica gel surface. The analytical potential of the method is demonstrated by the compositional mapping of a native GM3 (II(3)-alpha-Neu5Ac-LacCer) ganglioside mixture from cultured Chinese hamster ovary cells. The analysis is characterized by a high relative sensitivity, allowing the simultaneous detection of various major and minor GM3 species directly from individual HPTLC analyte bands. The lateral resolution of the direct HPTLC-MALDI-MS analysis is defined by the laser focus diameter of currently approximately 200 microm. This allows one to determine mobility profiles of individual species with a higher resolution than by reading off the chromatogram by optical absorption. The fluorescent dye primuline was, furthermore, successfully tested as a nondestructive, MALDI-compatible staining agent.

  16. (AJST) COMPARISON OF THIN LAYER CHROMATOGRAPHY (TLC)

    African Journals Online (AJOL)

    Administrator

    used for gas chromatographic determination. Soil: Triplicate soil samples (50 g), which had been sieved through 2mm mesh, were soxhlet extracted for 5 hours with 250 ml methanol. A 50 ml aliquot of methanol extract was evaporated to dryness in a rotary evaporator and the residue taken up in 1ml methanol: water mixture ...

  17. Quantitative characterization of tissue globotetraosylceramides in a rat model of polycystic kidney disease by PrimaDrop sample preparation and indirect high-performance thin layer chromatography-matrix-assisted laser desorption/ionization-time-of-flight-mass spectrometry with automated data acquisition.

    Science.gov (United States)

    Ruh, Hermelindis; Sandhoff, Roger; Meyer, Björn; Gretz, Norbert; Hopf, Carsten

    2013-07-02

    Glycosphingolipids (GSL) have been associated with a variety of diseases, including cancer and autosomal dominant polycystic kidney disease (ADPKD). In contrast to glucosylceramide and gangliosides, alterations in complex neutral GSLs such as globotetraosylceramide (Gb4Cer) have not been investigated in ADPKD yet, and mass spectrometry analysis of Gb4Cer from tissue extracts remains challenging. To this end, we introduce PrimaDrop as an improved and widely applicable sample preparation method for automated matrix-assisted laser desorption/ionization-mass spectrometry (MALDI-MS) analysis of lipid extracts, which promotes homogeneous cocrystallization and enables relative quantification by indirect thin layer chromatography (TLC)-MALDI-time-of-flight (TOF)-MS against an internal bradykinin standard. Application of the method for detailed investigation of Gb4Cer isoforms in kidneys of an ADPKD rat model revealed increased levels of sphingoid base-containing isoforms in cystic kidneys, whereas changes were subtle for Gb4Cer-containing phytosphingoid bases. We furthermore established an absolute LC-ESI-MS/MS quantification method and demonstrate that absolute quantities of Gb4Cer correlate well with relative quantities obtained by indirect TLC-MALDI-TOF-MS. Taken together, our study proposes an effective sample preparation method for automated analysis of lipid extracts and TLC eluates and suggests that indirect high-performace (HP)TLC-MALDI-TOF-MS with automated data acquisition is a viable option for analysis of neutral glycosphingolipids and that Gb4Cer may play a role in the pathogenesis of ADPKD.

  18. Estabilidad por cromatografía en capa delgada de mezclas de tinturas de Quassia amara y Maytenus ilicifolia Stability by thin-layer chromatography from Quassia amara and Maytenus ilicifolia tinctures

    Directory of Open Access Journals (Sweden)

    Eneyda Sieres Pedraja

    2009-12-01

    Full Text Available Una línea de investigación que ha tomado auge en los últimos tiempos, es aquella que se refiere a los productos fitoterapéuticos, por lo que se hizo necesaria una evaluación integral para su posterior utilización. Este trabajo describe un método por cromatografía en capa delgada, para evaluar la estabilidad de tinturas obtenidas a partir de un proceso de percolación de 2 plantas de origen brasileño: Quassia amara y Maytenus ilicifolia. El estudio se realizó teniendo en cuenta 3 temperaturas de almacenamiento: refrigeración, ambiente y 40 ºC, durante un tiempo de 90 días. Se seleccionaron las condiciones cromatográficas, se determinó el límite de detección y se demostró la selectividad del método, para lo cual se sometió el extracto a 4 condiciones de estrés. Se usó como fase móvil n-butanol-acido acético-agua (4:1:5 y como revelador la luz ultravioleta a una l de 366 nm. Los mejores resultados se observan cuando el extracto analizado se conserva en refrigeración durante el tiempo de estudio. Bajo condiciones de estrés, solo existen resultados favorables cuando es expuesto a la luz ultravioleta. Se establece como límite de detección el correspondiente a 7 µL.In past years, a research field with boom is that related to phytotherapeutical products, being necessary an integral research for its latter utilization. Present paper describes a thin layer chromatography (TLC method to assess the stability of tinctures obtained from a percolation process of two Brazilian plants: Quassia amara and Maytenus ilicifolia. Study took into account three storage temperatures: refrigeration, room-temperature and at 40 ºC during 90 days. Chomatographic conditions were selected, detection limit was determined, and method selectivity was demonstrated where the extract undergoes four stress-conditions. As a mobile phase we used n-butanol-acetic acid-water (4:1:5, and as UV at a l of 366 nm. The better results are obtained when analyzed

  19. Ocorrência de aflatoxinas em arroz consumido por militares do Exército Brasileiro por cromatografia em camada delgada e cromatografia líquida de alta eficiência Incidence of aflatoxins in rice to be consumed by militaries in the brazilian army by thin layer chromatography and high performance liquid chromatography methods

    Directory of Open Access Journals (Sweden)

    Jader Oliveira da Silva

    2008-08-01

    November 2003 to febuary 2004 when the incidence of aflatoxins B1, B2, G1 and G2 was measured by thin layer chromatography (TLC and high performance liquid chromatography (HPLC methods. This work had the aim of comparing the thin layer chromatography and high performance liquid chromatography techniques and contributed for the quality control of the foods to be consumed by militaries of the Brazilian army, concerning the control of the aflatoxins levels. From a total of 30 samples were tested performed by tlc, no aflatoxin was detected. From 26 samples, analysed trough high performance liquid chromatography, 6 (23, 07% presented positive results for aflatoxin B1 with 0, 54 2, 04 µg/kg and, 1 (3, 84% presented a positive result for aflatoxins B2 with 1, 84 µg/kg.

  20. Effective separation and analysis of E- and Z-guggulsterones in Commiphora mukul resin, guggulipid and their pharmaceutical product by high performance thin-layer chromatography-densitometric method.

    Science.gov (United States)

    Musharraf, Syed Ghulam; Iqbal, Naveed; Gulzar, Umair; Ali, Azhar; Choudhary, Muhammad Iqbal; Atta-Ur-Rahman

    2011-09-10

    A high performance thin-layer chromatographic (HPTLC) method for the simultaneous determination of the hypolipidemic agents, E- and Z-isomers of guggulsterone in Commiphora mukul resin, guggulipid (ethyl acetate extract of resin), and its pharmaceutical formulation, was developed. The developed system was efficient enough to separate both isomers from their conger, 17,20-dihydroguggulsterone. HPTLC glass plates, pre-coated with silica gel 60F-254, were used as a stationary phase. The mobile phase consisted of toluene:acetone (9.3:0.7, v/v) which gave well resolved spots for E- and Z-guggulsterones (R(f): 0.52±0.01, and 0.67±0.01, respectively) following double development of chromatoplate with the same mobile phase under unsaturated conditions. The analyte stability towards the developed chromatographic procedure was also investigated by two-dimensional (2D) HPTLC analysis. 17,20-Dihydroguggulsterone (3) was identified by the electrospray ionization quadrupole time-of-flight tandem mass spectrometry (ESI-QTOF-MS/MS) analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Showing Its Colors. Thin-Layer Chromatographic Detection of Cannabinoid Metabolites.

    Science.gov (United States)

    Bonicamp, Judith M.

    1986-01-01

    Describes a chemistry laboratory experiment in which thin-layer chromatography (TLC) is used to analyze urine specimens containing metabolites of the drug tetrahydro-cannabinol, which comes from the marijuana plant. The materials needed to conduct the experiment are listed, and the procedure and expected results are outlined. (TW)

  2. Plant-determined variation in the cardenolide content, thin-layer chromatography profiles, and emetic potency of monarch butterflies,Danaus plexippus reared on the milkweed,Asclepias eriocarpa in California.

    Science.gov (United States)

    Brower, L P; Seiber, J N; Nelson, C J; Lynch, S P; Tuskes, P M

    1982-03-01

    This paper is the first in a series on cardenolide fingerprinting of the monarch butterfly. New methodologies are presented which allow both qualitative and quantitative descriptions of the constituent cardenolides which these insects derive in the wild from specificAsclepias foodplants. Analyses of thin-layer Chromatographic profiles ofAsclepias eriocarpa cardenolides in 85 individual plant-butterfly pairs collected at six widely separate localities in California indicate a relatively invariant pattern of 16-20 distinct cardenolides which we here define as theAsclepias eriocarpa cardenolide fingerprint profile. Cardenolide concentrations vary widely in the plant samples, but monarchs appear able to regulate total storage by increasing their concentrations relative to their larval host plant when reared on plants containing low concentrations, and vice versa. Forced-feeding of blue jays with powdered butterfly and plant material and with one of the constituent plant cardenolides, labriformin, established that theA. eriocarpa cardenolides are extremely emetic, and that monarchs which have fed on this plant contain an average of 16 emetic-dose fifty (ED50) units. The relatively nonpolar labriformin and labriformidin in the plant are not stored by the monarch but are metabolized in vivo to desglucosyrioside which the butterfly does store. This is chemically analogous to the way in which monarchs and grasshoppers metabolize another series of milkweed cardenolides, those found inA. curassavica. It appears that the sugar moiety through functionality at C-3' determines which cardenolides are metabolized and which are stored. The monarch also appears able to store several lowR f cardenolides fromA. eriocarpa without altering them. Differences in the sequestering process in monarchs and milkweed bugs (Oncopeltus) may be less than emphasized in the literature. The monarch is seen as a central organism involved in a coevolutionary triad simultaneously affecting and affected

  3. Intralaboratory optimization and validation of a method for patulin determination in grapes by Thin-Layer Chromatography Otimização e validação intralaboratorial de método para a determinação de patulina em uva por Cromatografia em Camada Delgada

    Directory of Open Access Journals (Sweden)

    Renata Cabrera de Oliveira

    2007-06-01

    Full Text Available The aim of this work was to optimize and validate, by intralaboratorial procedures, a method for the determination of patulin in grapes by thin-layer chromatography. The steps of extraction, cleanup, detection and quantification were optimized. For the validation of the method, recovery assays with standard solutions and artificially contaminated samples were carried out. The mean recovery and the variation coefficient were 65.4% and 7.58%, respectively. The optimized conditions were: 50 mL of grape juice, three extraction stages (with 100 mL of ethyl acetate in the first stage and 50 mL in second and third stages, and 100 µL of ethanol to solubilize the extract. The solvent-system used was toluene - ethyl acetate - formic acid (6:3:1, and 0.5% MBTH in 5% formic acid was sprayed on the plates to intensify the fluorescence. The visual detection and quantification limits were 7.44 ng and 15.87 µg.kg-1, respectively. The optimized and validated method demonstrated sufficient efficiency for adoption in the monitoring of patulin in grape.O objetivo deste trabalho foi otimizar e validar, por procedimentos intralaboratoriais, um método de determinação de patulina em uva por cromatografia em camada delgada. Foram realizados testes de otimização das etapas de extração, limpeza, detecção e quantificação. Para validação do método foram realizados ensaios de recuperação com soluções padrões e amostras artificialmente contaminadas. A recuperação e o coeficiente de variação foram 65,4% e 7,58%, respectivamente. As condições otimizadas foram: 50 mL do suco da uva; três etapas de extração, 100 mL de acetato de etila na primeira etapa e 50 mL na segunda e terceira etapas; 100 µL de etanol para solubilizar o extrato; a fase móvel tolueno-acetato de etila-ácido fórmico (6:3:1 e o revelador o MBTH 0,5% em ácido fórmico 5%. O limite de detecção visual foi de 7,44 ng e o de quantificação de 15,87 µg/kg. O método otimizado e

  4. Risks and possibilities in patch testing with contaminated personal objects: usefulness of thin-layer chromatograms in a patient with acrylate contact allergy from a chemical burn.

    Science.gov (United States)

    Isaksson, Marléne; Zimerson, Erik

    2007-08-01

    We report a case of a chemical burn from dipropylene glycol diacrylate (DPGDA) spilt on working shoes, followed by active sensitization, thus giving an occupational allergic contact dermatitis on the patient's dorsal feet. Diagnostic tests included patch testing with acetone extracts made from the different shoe layers and thin-layer chromatograms. An invisible spot on the thin-layer chromatography plate gave a test eczema and was further investigated with gas chromatography-mass spectrometry. DPGDA was detected in the spot.

  5. Thermal analysis of thin layer boilover

    Energy Technology Data Exchange (ETDEWEB)

    Kozanoglu, Bulent [Universidad de las Americas, Puebla (Mexico); Mechanical Engineering Department, Cholula, Puebla (Mexico); Ferrero, Fabio; Munoz, Miguel; Arnaldos, Josep; Casal, Joaquim [Universitat Politecnica de Catalunya, Barcelona (Spain)

    2008-10-15

    A mathematical model is developed to simulate the thin layer boilover phenomenon. This model takes into account convective currents as well as conduction and radiation absorption through the fuel layer and is resolved numerically employing a scheme of Runge-Kutta, combined with the numerical method of lines. Solutions of the model showed a good agreement with the experimental data, both from this work and by other authors, demonstrating the importance of the convective currents. The model provided velocities of these currents, of the same order of magnitude as the values reported in the technical literature. Thickness of the remaining fuel and the interface temperature are correctly calculated by the model, allowing the prediction of the time required for the boilover to start. (orig.)

  6. Suitability of thin-layer chromatography-flame ionization detection with regard to quantitative characterization of different fossil fuel products. 1. FID performances and response of pure compounds related to fossil fuel products

    Energy Technology Data Exchange (ETDEWEB)

    Cebolla, V.L.; Vela, J.; Membrado, L.; Ferrando, A.C. [CSIC, Zaragoza (Spain). Inst. de Carboquimica, Dept. de Procesos Quimicos

    1998-10-01

    The performance of a modern TLC-FID system (which includes the newest detector configuration) was tested on polycyclic aromatic compound standards and related compounds as a preliminary step to evaluate its suitability for quantitative hydrocarbon group type analysis of different coal and petroleum products. FID linearity was evaluated as a function of sample load and scan speed for high-molecular-weight and semi-volatile standards. TLC-FID response factors for compounds of several homologous series were studied in order to differentiate effects of volatility from those exclusively due to the chemical nature concerning FID response. Criteria are developed for the accurate application of TLC-FID to fossil fuel samples. Measurements of chromarod temperatures were carried out in order to evaluate whether an evaporation of compounds outside the H{sub 2} flame might take place. 10 refs., 3 figs., 4 tabs.

  7. Thin-Layer Fuel Cell for Teaching and Classroom Demonstrations

    Science.gov (United States)

    Shirkhanzadeh, M.

    2009-01-01

    A thin-layer fuel cell is described that is simple and easy to set up and is particularly useful for teaching and classroom demonstrations. The cell is both an electrolyzer and a fuel cell and operates using a thin layer of electrolyte with a thickness of approximately 127 micrometers and a volume of approximately 40 microliters. As an…

  8. Thin-layer chromatographic (TLC) separations and bioassays of plant extracts to identify antimicrobial compounds.

    Science.gov (United States)

    Kagan, Isabelle A; Flythe, Michael D

    2014-03-27

    A common screen for plant antimicrobial compounds consists of separating plant extracts by paper or thin-layer chromatography (PC or TLC), exposing the chromatograms to microbial suspensions (e.g. fungi or bacteria in broth or agar), allowing time for the microbes to grow in a humid environment, and visualizing zones with no microbial growth. The effectiveness of this screening method, known as bioautography, depends on both the quality of the chromatographic separation and the care taken with microbial culture conditions. This paper describes standard protocols for TLC and contact bioautography with a novel application to amino acid-fermenting bacteria. The extract is separated on flexible (aluminum-backed) silica TLC plates, and bands are visualized under ultraviolet (UV) light. Zones are cut out and incubated face down onto agar inoculated with the test microorganism. Inhibitory bands are visualized by staining the agar plates with tetrazolium red. The method is applied to the separation of red clover (Trifolium pratense cv. Kenland) phenolic compounds and their screening for activity against Clostridium sticklandii, a hyper ammonia-producing bacterium (HAB) that is native to the bovine rumen. The TLC methods apply to many types of plant extracts and other bacterial species (aerobic or anaerobic), as well as fungi, can be used as test organisms if culture conditions are modified to fit the growth requirements of the species.

  9. Comparison of thin layer chromatography (TLC) and gas ...

    African Journals Online (AJOL)

    The fate of propoxur in a cocoa ecosystem has been studied using TLC and GC. Residues of propoxur as determined by both TLC and GC were not significantly different. TLC analysis of propoxur residues in soil, cocoa leaves and pods may not need any rigorous clean up since residues measured from cleaned and ...

  10. PRELIMINARY PHYTOCHEMICAL INVESTIGATION AND THIN LAYER CHROMATOGRAPHY OF RHEUM EMODI

    OpenAIRE

    Mir Ashfaq Ahmad; K. W. Shah; Showkat Ahmad Wani

    2012-01-01

    Preliminary phytochemical investigation of aqueous and methanolic rhizome extracts of Rheum emodi followed by their TLC profiling were carried out. Phytochemical analysis reveals the presence of diverse groups of phytoconstituents in two different extracts (aqueous and methanolic rhizome extracts). Chemical constituents also show different Rf values in two different solvent systems.

  11. Phytochemical screening and thin layer chromatography of the ...

    African Journals Online (AJOL)

    Phytochemical constituents of the leaves of Khaya senegalensis (dry zone mahogany) were determined in petroleum ether, chloroform, acetone and ethanol extracts. The screening revealed the presence of flavonoids, carbohydrates, glycosides, saponins, tannins, alkaloids and anthraquinones. Saponins and cardiac ...

  12. Development of high performance thin layer chromatography for ...

    African Journals Online (AJOL)

    HPTLC) system with WinCATS software was used. Freshly prepared solutions in methanol were spotted on HPTLC silica gel 60F254 plates. The mobile phase was composed by 20 mL of toluene and 10 mL of methanol, both analytical grades.

  13. High-performance thin-layer chromatography (HPTLC)

    National Research Council Canada - National Science Library

    Srivastava, ManMohan

    2011-01-01

    ... on HPTLC fundamentals: principle, theory, understanding; instrumentation: implementation, optimization, validation, automation and qualitative and quantitative analysis; applications: phytochemical analysis, biomedical analysis, herbal drug quantification, analytical analysis, finger print analysis and potential for hyphenation: HPTLC future to combinat...

  14. Comparação das técnicas de cromatografia em camada delgada e ELISA na quantificação de aflatoxinas em amostras de milho Comparison of thin layer chromatography and ELISA techniques in the quantification of aflatoxins in corn samples

    Directory of Open Access Journals (Sweden)

    Marize Silva OLIVEIRA

    2000-12-01

    Full Text Available A comparação das técnicas de Enzyme Linked Immunosorbent Assay (ELISA e cromatografia em camada delgada (CCD por quantificação visual e densitométrica foi utilizada na determinação de aflatoxina total, em amostras de milho naturalmente contaminadas. Os teores de aflatoxina total encontrados pelas técnicas de CCD e ELISA, apresentaram maior freqüência na faixa de 0-30 mig/kg e acima de 300 mig/kg. Os resultados das amostras apresentaram coeficiente de variação concentrados abaixo de 20, 30 e 40% para a técnica de ELISA e CCD com quantificação densitométrica e visual, respectivamente. Os coeficientes de correlação foram altamente significativos para as relações entre as quantificações visual e densitométrica (r = 0,9219; t = 26,36; p Two methods, enzyme linked immunosorbent assay (ELISA and thin layer chromatography (TLC by visual and densitometric, were compared for determination of aflatoxins in corn samples. The highest incidence of total aflatoxin detected by those methods were ranged from 0-30 mug/kg and above 300 mug/kg. For aflatoxins B2, G1, G2 the levels were ranged from 0-30mug/kg. The samples results showed variation coefficient below of 20, 30 and 40% for ELISA and CCD with densitometric and visual quantification, respectively. The correlation coefficients were highly significative for the relation between visual quantification and densitometric (r = 0,9219; t = 28,36; p<0,001, ELISA and visual quantification (r =0,8277; t = 17,58; p< 0,001, ELISA e quantification densitometric (r = 0,7373; t=13,01; p< 0,001, in the total aflatoxin detemination of all corn samples. confirming the equivalence of the studied methods.

  15. Quantitative thin layer chromatographic analysis of the saponins in tea seed meal.

    Science.gov (United States)

    Chaicharoenpong, Chanya; Petsom, Amorn

    2009-01-01

    The defatted seed meal of Camellia oleifera Abel., which contains saponins, is used extensively in aquaculture to eliminate unwanted fish and harmful insects during the cultivation of prawns, and as a molluscicide to control Pomacea canaliculata Lamarck. For the quality control of such tea seed meal products, a method for the determination of saponin content is required. To develop a simple, sensitive and specific method for the quantitative determination of saponins in tea seed meal using high-performance thin layer chromatography and densitometry. Powdered tea seed meal samples were extracted with methanol, filtered, evaporated to dryness and the residue taken up in methanol. Samples, together with methanolic solutions of saponin standard, were analysed by HPTLC on silica gel layers eluted with ethyl acetate:methanol:water (6:3:1.5, v/v/v) and detected at 214 nm. The amounts of saponins were determined from the respective calibration curves obtained by plotting the concentrations of saponin standard against peak area. Tea saponin peaks were detected at about R(f )0.40. Good linearity was observed in the range of 0.9-22.2 microg/spot with a correlation coefficient of 0.9978. The limits of detection and quantification were 0.87 and 2.90 microg/spot, respectively. The content of tea saponins in 10 tested samples was found to be between 13.1 and 21.1% w/w. The assay proved to be a specific, sensitive and inexpensive method for the quality control of saponins in tea seed meal. Copyright (c) 2009 John Wiley & Sons, Ltd.

  16. Degradation of dansyl polyamines on high-performance thin-layer chromatographic plates.

    Science.gov (United States)

    Rustenbeck, I; Löptien, D; Lenzen, S

    1995-05-05

    Using high-performance thin-layer chromatography with in situ quantitation to measure dansylated polyamines in the range of 1-20 pmol, we found that dansylated polyamines apparently react with the silica gel of the plates. The fluorescence of the dansyl polyamines diminished with increase in the time interval between application of a sample to the plate and start of the chromatographic separation. Conversely, the fluorescence at the site of application increased with the length of the time interval, indicating the formation of polar reaction products. If this reaction is not accounted for, considerable errors in quantitation of dansyl polyamines may occur.

  17. Desarrollo y validación de un método por cromatografía en capa delgada para los estudios de estabilidad del naproxeno Development and validation of a thin-layer chromatography method for stability studies of naproxen

    Directory of Open Access Journals (Sweden)

    Yaslenis Rodríguez Hernández

    2011-12-01

    satisfactory. A thin-layer chromatography-based method was developed as well as the best chromatographic conditions were selected. GF254 silica gel plates and ultraviolet developer at 254 nm were employed. Three solvent systems were evaluated of which A made up of glacial acetic: tetrahydrofurane:toluene (3:9:90 v/v/vallowed adequate resolution between the analyte and the possible degradation products, with detection limit of 1 µg. The use of the suggested method was restricted to the identification of possible degradation products just for qualitative purposes and not as final test. The method proved to be sensitive and selective enough to be applied for the stated objective, according to the validation results.

  18. Mathematical Modelling of Thin Layer Dried Cashew Kernels | Asiru ...

    African Journals Online (AJOL)

    Seven different thin layer mathematical drying models were compared according to their coefficients of determination (R2) mean square error (MSE) and mean relative deviation modulus (P) to estimate drying curves. The effects of the drying air temperature and time on the drying model constants and coefficients were ...

  19. A Thin Layer Chromotographic (TLC) detection methodology for ...

    African Journals Online (AJOL)

    This paper presents a Thin Layer Chromatographic (TLC) detection methodology for the qualitative and quantitative determination of herbicides, using some local plants/grasses as part of an on-going method development for providing alternative cost-effective analytical procedure for screening pesticide residues. Out of the ...

  20. (AJST) THIN- LAYER DRYING OF DICED CASSAVA ROOTS

    African Journals Online (AJOL)

    opiyo

    accepted thin layer drying equations were fitted to the drying data of cassava cubes, and the Page model was found to agree with the ... The most common processing methods are direct sun- drying of peeled roots for days in to a ..... nature of solar radiation and the fact that the experiment was done continuously including ...

  1. Thin layer drying kinetics of amaranth (Amaranthus cruentus) grains ...

    African Journals Online (AJOL)

    An experimental solar tent dryer under natural convection was used to study thin layer drying kinetics of amaranth (Amaranthus cruentus) grains. Drying of grains in the dryer was carried out on a drying rack having two layers; top and bottom. The ambient temperature and relative humidity ranged from 22.6–30.4oC and ...

  2. Modeling of thin layer drying of tarragon (Artemisia dracunculus L.)

    NARCIS (Netherlands)

    ArabHosseini, A.; Huisman, W.; Boxtel, van A.J.B.; Mueller, J.

    2009-01-01

    The drying behavior of tarragon leaves as well as chopped plants were evaluated at air temperatures ranging from 40 to 90 °C, at various air relative humidities and a constant air velocity of 0.6 m/s. The experimental data was fitted to a number of thin layer drying equations. The equations were

  3. Standard flow liquid chromatography for shotgun proteomics in bioenergy research

    Directory of Open Access Journals (Sweden)

    Susana M. González Fernández-Niño

    2015-04-01

    Full Text Available Over the past ten years the bioenergy and biofuels field has realized significant achievements that have encouraged many follow on efforts centered on biosynthetic production of fuel-like compounds. Key to the success of these efforts has been transformational developments in feedstock characterization and metabolic engineering of biofuel-producing microbes. Lagging far behind these advancements are analytical methods to characterize and quantify systems of interest to the bioenergy field. In particular the utilization of proteomics, while valuable for identifying novel enzymes and diagnosing problems associated with biofuel-producing microbes, is limited by a lack of robustness and limited throughput. Nano-flow liquid chromatography coupled to high-mass accuracy, high-resolution mass spectrometers has become the dominant approach for the analysis of complex proteomic samples, yet such assays still require dedicated experts for data acquisition, analysis, and instrument upkeep. The recent adoption of standard flow chromatography (ca. 0.5 mL/min for targeted proteomics has highlighted the robust nature and increased throughput of this approach for sample analysis. Consequently, we assessed the applicability of standard flow liquid chromatography for shotgun proteomics using samples from Escherichia coli and Arabidopsis thaliana, organisms commonly used as model systems for lignocellulosic biofuels research. Employing 120 minute gradients with standard flow chromatography we were able to routinely identify nearly 800 proteins from E. coli samples, while for samples from Arabidopsis over 1,000 proteins could be reliably identified. An examination of identified peptides indicated that the method was suitable for reproducible applications in shotgun proteomics. Standard flow liquid chromatography for shotgun proteomics provides a robust approach for the analysis of complex samples. To the best of our knowledge this study represents the first attempt

  4. Ion Exchange and Thin Layer Chromatographic Separation and Identification of Amino Acids in a Mixture: An Experiment for General Chemistry and Biotechnology Laboratories

    Science.gov (United States)

    Brunauer, Linda S.; Caslavka, Katelyn E.; Van Groningen, Karinne

    2014-01-01

    A multiday laboratory exercise is described that is suitable for first-year undergraduate chemistry, biochemistry, or biotechnology students. Students gain experience in performing chromatographic separations of biomolecules, in both a column and thin layer chromatography (TLC) format. Students chromatographically separate amino acids (AA) in an…

  5. A contribution to the determination of aflatoxin B1, quinine hydrochloride and L(+)-ascorbic acid in foodstuffs by quantitative in situ thin-layer chromatographic analysis

    NARCIS (Netherlands)

    Beljaars, P.R.

    1974-01-01

    The application of quantitative thin-layer chromatography (TLC) involving in situ spectrodensitometric measurements with a flying-spot densitometer is described in this study for the analysis of aflatoxin B 1 , quinine hydrochloride

  6. Physico-chemical standardization of Sitopaladi churna.

    Science.gov (United States)

    Makhija, Inder Kumar; Shreedhara, Chandrashekara Shastry; Ram, Holavana Hally Nanjundaiah Setty Aswatha

    2012-01-01

    Standardization of a compound Ayurvedic formulation is a critical and essential issue to be considered in assuring the therapeutic efficacy and safety and to rationalize their use in the health care. Sitopaladi churna is a reputed polyherbal formulation of Ayurveda. It is prescribed for the treatment of pleurodynia, intercostal neuralgia, cold, cough associated with bronchitis, pneumonia, tuberculosis, viral respiratory infection, and in pharyngeal and chest congestion. The present study aimed at physico-chemical standardization of in-house and two marketed brands of Sitopaladi churna. In our investigation, in-house churna and two commercial brands of Sitopaladi churna were standardized based on powder microscopy, physico-chemical evaluations, thin layer chromatography (TLC) and high performance thin layer chromatography (HPTLC) finger printing as per standard procedures. The set parameters were sufficient to evaluate the churna based on various physico-chemical parameters. The data evolved can be adopted for laying down the standards for the manufacturing units of Sitopaladi churna.

  7. Copper (II) Schiff base complexes and their mixed thin layers with ...

    Indian Academy of Sciences (India)

    Copper(II) Schiff base complexes and their mixed thin layers with ZnO nanoparticles. MAGDALENA ... Keywords. Thin layer; ZnO nanoparticles; copper complexes; AFM; SEM; fluorescence. ... Zinc oxide was synthesized using a simple homogeneous precipitation method with zinc acetate as a starting material. Thin layers ...

  8. Thin layer chromatographic analysis of some common over the counter (OTC cough–cold preparations

    Directory of Open Access Journals (Sweden)

    Manpreet Kaur Chahal

    2016-12-01

    Full Text Available In the present study, potential utility of thin layer chromatography to differentiate some common OTC cough–cold preparations was evaluated. Twenty solvent systems were examined from which a solvent systems A comprising methanol:ammonia in the ratio of 100:1.5 (v/v and B comprising chloroform:methanol in the ratio of 90:10 (v/v were found to be most suitable as it showed a high degree of separation of different components of these preparations. It was also found that iodine fuming technique is the best visualizing method for examining the TLC chromatograms of these drug samples prior to subsequent instrumental analysis.

  9. Thin-Layer Solutions of the Helmholtz and Related Equations

    KAUST Repository

    Ockendon, J. R.

    2012-01-01

    This paper concerns a certain class of two-dimensional solutions to four generic partial differential equations-the Helmholtz, modified Helmholtz, and convection-diffusion equations, and the heat conduction equation in the frequency domain-and the connections between these equations for this particular class of solutions.S pecifically, we consider thin-layer solutions, valid in narrow regions across which there is rapid variation, in the singularly perturbed limit as the coefficient of the Laplacian tends to zero.F or the wellstudied Helmholtz equation, this is the high-frequency limit and the solutions in question underpin the conventional ray theory/WKB approach in that they provide descriptions valid in some of the regions where these classical techniques fail.E xamples are caustics, shadow boundaries, whispering gallery, and creeping waves and focusing and bouncing ball modes.It transpires that virtually all such thin-layer models reduce to a class of generalized parabolic wave equations, of which the heat conduction equation is a special case. Moreover, in most situations, we will find that the appropriate parabolic wave equation solutions can be derived as limits of exact solutions of the Helmholtz equation.W e also show how reasonably well-understood thin-layer phenomena associated with any one of the four generic equations may translate into less well-known effects associated with the others.In addition, our considerations also shed some light on the relationship between the methods of matched asymptotic, WKB, and multiple-scales expansions. © 2012 Society for Industrial and Applied Mathematics.

  10. Microstructure of bidisperse ferrofluids in a thin layer

    Energy Technology Data Exchange (ETDEWEB)

    Minina, E. S., E-mail: alla2307@gmail.com; Muratova, A. B. [Ural Federal University, Department of Mathematical Physics (Russian Federation); Cerda, J. J. [Campus University de les Illes Balears, Institute for Cross-Disciplinary Physics and Complex Systems (Spain); Kantorovich, S. S., E-mail: sue.kantorovich@usu.ru [Ural Federal University, Department of Mathematical Physics (Russian Federation)

    2013-03-15

    In this work we present a characterization of the bidisperse ferrofluid microstructures that appear in thin layers of ferrofluid. These layers have been studied by a combination of Langevin dynamics simulations and density functional theory. Our results allow us to compare the microstructures that exist in quasi-two-dimensional ferrofluid nanolayers with the microstructures found in three-dimensional bidisperse ferrofluids. Furthermore, our results allow us to explain the influence of the geometry of the sample on the topology and size-distribution of the observed aggregates of magnetic nanoparticles.

  11. Intoxicação em cães e gatos: diagnóstico toxicológico empregando cromatografia em camada delgada e cromatografia líquida de alta pressão com detecção ultravioleta em amostras estomacais Intoxication in dogs and cats: toxicological diagnosis using thin layer chromatography and high pressure liquid chromatography with ultraviolet detection in stomach samples

    Directory of Open Access Journals (Sweden)

    Rachel Picada Bulcão

    2010-05-01

    óticos mais envolvidos nessas intoxicações.The pesticides and rodenticides are responsible for several human and animal intoxications. Preliminary data suggest that the illegal use of these compounds to poison small animals is a common practice in the central region of the Rio Grande do Sul state. The Laboratory of Toxicology received samples, of cases in which the main suspected cause of death is poisoning by pesticides or exogenous rodenticides (licit and illicit. The aim of this study was show the survey of small animals poisoned and analyzed by LATOX during the period of 2004 to 2008 identifying the xenobiotics by optimized analytical methods, including screening by thin-layer chromatography (TLC and a possible confirmation by high performance liquid chromatography - ultraviolet detection (HPLC-UV. In this period 68 samples were analyzed from small poisoned animals. The biological samples analyzed were stomach and stomach content and the TLC permitted carbamates, warfarin and stricnine identification. This proved to be an efficient and adequate technique for this purpose, relatively fast, inexpensive and with low matrix interference. The screening by HPLC for N-methyl carbamates was also realized: aldicarb, carbaryl, carbofuran and propoxur. The analysis showed that the main toxic agent found was aldicarb (chumbinho, responsible for 39.7% of poisoning (27 cases, followed by stricnine (6 cases, warfarin (3 cases and sodium monofluoracetate (1 case. Thus, the 'chumbinho' was the main agent involved in dogs and cats poisoning in the central region of the state, during the analyzed period. The analytical methods TLC and HPLC can be used efficiently in laboratorial routine for identification and confirmation of xenobiotics involved in these poisonings.

  12. Surface Morphology of Fe(III)-Porphyrin Thin Layers as Characterized by Atomic Force Microscopy

    OpenAIRE

    Utari Utari; Kusumandari Kusumandari; Budi Purnama; Mudasir Mudasir; Kamsul Abraha

    2016-01-01

    Surface morphology of Fe(III)–porphyrin thin layers was studied using atomic force microscopy. The thin layer samples used in these experiments were deposited by spin coating methods on indium–tin-oxide substrates at room temperature under atmospheric conditions. Variations of thin layer of Fe(III)-porphyrin were done by modifying the rotational speed and the concentration of the solution. The experimental results demonstrated that the Fe(III)–porphyrin layers were observed as discrete nanomo...

  13. Thin layer modelling of Gelidium sesquipedale solar drying process

    Energy Technology Data Exchange (ETDEWEB)

    Ait Mohamed, L. [Laboratoire d' Energie Solaire et des Plantes Aromatiques et Medicinales, Ecole Normale Superieure, BP 2400, Marrakech (Morocco); Faculte des Sciences Semlalia, BP 2390, Marrakech (Morocco); Ethmane Kane, C.S. [Faculte des Sciences de Tetouan, BP 2121, Tetouan (Morocco); Kouhila, M.; Jamali, A. [Laboratoire d' Energie Solaire et des Plantes Aromatiques et Medicinales, Ecole Normale Superieure, BP 2400, Marrakech (Morocco); Mahrouz, M. [Faculte des Sciences Semlalia, BP 2390, Marrakech (Morocco); Kechaou, N. [Ecole Nationale d' Ingenieurs de Sfax, BPW 3038 (Tunisia)

    2008-05-15

    The effect of air temperature and air flow rate on the drying kinetics of Gelidium sesquipedale was investigated in convective solar drying. Drying was conducted at 40, 50 and 60 C. The relative humidity was varied from 50% to 57%, and the drying air flow rate was varied from 0.0277 to 0.0833 m{sup 3}/s. The expression for the drying rate equation is determined empirically from the characteristic drying curve. Thirteen mathematical models of thin layer drying are selected in order to estimate the suitable model for describing the drying curves. The two term model gives the best prediction of the drying curves and satisfactorily describes the drying characteristics of G. sesquipedale with a correlation coefficient R of 0.9999 and chi-square ({chi}{sup 2}) of 3.381 x 10{sup -6}. (author)

  14. Investigation of Processes and Factors Regulating the Generation, Maintenance and Breakdown of Bioluminescent Thin Layers

    National Research Council Canada - National Science Library

    Widder, Edith

    2001-01-01

    .... Katz's submersible holographic camera mounted on the upper work platform. Thin layers were located using real-time sensor feedback from intensified video recordings of stimulated bioluminescence...

  15. Copepod Behavior in Thin Layers of Toxic Algae

    Science.gov (United States)

    Webster, D. R.; True, A. C.; Weissburg, M. J.; Yen, J.

    2016-02-01

    Cryptic blooms of toxic phytoplankton were modeled in a custom thin layer flume for behavioral assays with calanoid copepods. Acartia tonsa and Temora longicornis were exposed to thin layers of exudates from the toxic dinoflagellate Karenia brevis (1 - 10,000 cells/mL). Planar laser-induced fluorescence (PLIF) was used to quantify the spatial structure of the layer allowing for correlation of behavioral responses with toxin levels. Both species explicitly avoided the exudate layer and the vicinity of the layer. Measures of path kinematics (swimming speed, turn frequency) by location (in-layer vs. out-of-layer) and exposure (pre-contact vs. post-contact) revealed some similarities, but also significant differences, in trends for each species. A. tonsa significantly increased swimming speed and swimming speed variability in the exudate layer and post-contact, whereas T. longicornis slightly increased both in-layer and slightly reduced both post-contact. Both species increased turn frequency in-layer and post-contact with increasing K. brevis exudate concentration. Path fractal geometry indicated that A. tonsa trajectories became more diffuse/sinuous and T. longicornis trajectories became more linear/ballistic (trending effects). Regression analyses revealed that the rate of change of behavior with increasing exudate concentration for A. tonsa was three to fifty times that of T. longicornis depending on the parameter considered. The results suggested that toxic K. brevis can essentially eliminate top-down grazer control, another sinister means by which it gains a competitive advantage over the local phytoplankton taxa.

  16. Femtosecond pulsed laser deposition of biological and biocompatible thin layers

    Energy Technology Data Exchange (ETDEWEB)

    Hopp, B. [Hungarian Academy of Sciences, University of Szeged, Research Group on Laser Physics, Dom ter 9, H-6720 Szeged (Hungary)]. E-mail: bhopp@physx.u-szeged.hu; Smausz, T. [Hungarian Academy of Sciences, University of Szeged, Research Group on Laser Physics, Dom ter 9, H-6720 Szeged (Hungary); Kecskemeti, G. [Department of Optics and Quantum Electronics, University of Szeged, Dom ter 9, H-6720 Szeged (Hungary); Klini, A. [Institute of Electronic Structure and Laser (I.E.S.L.), Foundation for Research and Technology-Hellas (F.O.R.T.H.), P.O. Box 1527, GR-711 10 Heraklion, Crete (Greece); Bor, Zs. [Department of Optics and Quantum Electronics, University of Szeged, Dom ter 9, H-6720 Szeged (Hungary)

    2007-07-31

    In our study we investigate and report the femtosecond pulsed laser deposition of biological and biocompatible materials. Teflon, polyhydroxybutyrate, polyglycolic-acid, pepsin and tooth in the form of pressed pellets were used as target materials. Thin layers were deposited using pulses from a femtosecond KrF excimer laser system (FWHM = 450 fs, {lambda} = 248 nm, f = 10 Hz) at different fluences: 0.6, 0.9, 1.6, 2.2, 2.8 and 3.5 J/cm{sup 2}, respectively. Potassium bromide were used as substrates for diagnostic measurements of the films on a FTIR spectrometer. The pressure in the PLD chamber was 1 x 10{sup -3} Pa, and in the case of tooth and Teflon the substrates were heated at 250 deg. C. Under the optimized conditions the chemical structure of the deposited materials seemed to be largely preserved as evidenced by the corresponding IR spectra. The polyglycolic-acid films showed new spectral features indicating considerable morphological changes during PLD. Surface structure and thickness of the layers deposited on Si substrates were examined by an atomic force microscopy (AFM) and a surface profilometer. An empirical model has been elaborated for the description of the femtosecond PLD process. According to this the laser photons are absorbed in the surface layer of target resulting in chemical dissociation of molecules. The fast decomposition causes explosion-like gas expansion generating recoil forces which can tear off and accelerate solid particles. These grains containing target molecules without any chemical damages are ejected from the target and deposited onto the substrate forming a thin layer.

  17. A thin layer angiogenesis assay: a modified basement matrix assay for assessment of endothelial cell differentiation.

    Science.gov (United States)

    Faulkner, Ashton; Purcell, Robert; Hibbert, Andrew; Latham, Sally; Thomson, Scott; Hall, Wendy L; Wheeler-Jones, Caroline; Bishop-Bailey, David

    2014-12-05

    Basement matrices such as Matrigel™ and Geltrex™ are used in a variety of cell culture assays of anchorage-dependent differentiation including endothelial cell tube formation assays. The volumes of matrix recommended for these assays (approximately 150 μl/cm(2)) are costly, limit working distances for microscopy, and require cell detachment for subsequent molecular analysis. Here we describe the development and validation of a thin-layer angiogenesis (TLA) assay for assessing the angiogenic potential of endothelial cells that overcomes these limitations. Geltrex™ basement matrix at 5 μl/cm(2) in 24-well (10 μl) or 96-well (2 μl) plates supports endothelial cell differentiation into tube-like structures in a comparable manner to the standard larger volumes of matrix. Since working distances are reduced, high-resolution single cell microscopy, including DIC and confocal imaging, can be used readily. Using MitoTracker dye we now demonstrate, for the first time, live mitochondrial dynamics and visualise the 3-dimensional network of mitochondria present in differentiated endothelial cells. Using a standard commercial total RNA extraction kit (Qiagen) we also show direct RNA extraction and RT-qPCR from differentiated endothelial cells without the need to initially detach cells from their supporting matrix. We present here a new thin-layer assay (TLA) for measuring the anchorage-dependent differentiation of endothelial cells into tube-like structures which retains all the characteristics of the traditional approach but with the added benefit of a greatly lowered cost and better compatibility with other techniques, including RT-qPCR and high-resolution microscopy.

  18. Mathematical analogies in physics. Thin-layer wave theory

    Directory of Open Access Journals (Sweden)

    José M. Carcione

    2014-03-01

    Full Text Available Field theory applies to elastodynamics, electromagnetism, quantum mechanics, gravitation and other similar fields of physics, where the basic equations describing the phenomenon are based on constitutive relations and balance equations. For instance, in elastodynamics, these are the stress-strain relations and the equations of momentum conservation (Euler-Newton law. In these cases, the same mathematical theory can be used, by establishing appropriate mathematical equivalences (or analogies between material properties and field variables. For instance, the wave equation and the related mathematical developments can be used to describe anelastic and electromagnetic wave propagation, and are extensively used in quantum mechanics. In this work, we obtain the mathematical analogy for the reflection/refraction (transmission problem of a thin layer embedded between dissimilar media, considering the presence of anisotropy and attenuation/viscosity in the viscoelastic case, conductivity in the electromagnetic case and a potential barrier in quantum physics (the tunnel effect. The analogy is mainly illustrated with geophysical examples of propagation of S (shear, P (compressional, TM (transverse-magnetic and TE (transverse-electric waves. The tunnel effect is obtained as a special case of viscoelastic waves at normal incidence.

  19. Comparison of Two Detection Methods in Thin Layer ...

    African Journals Online (AJOL)

    komla

    The most important of such chromatographic techni-ques are gas chromatography (GC), high .... were air-dried and placed in a tank saturated with chlorine for 30 sec. The chlorine solution was made by ... the study of herbicides residue in the soil using the gas chromato-graphy method. By comparing the detection limit for ...

  20. Thin layer chromatographic analysis of food colorants from three morphotypes of annatto (Bixa orellana L.

    Directory of Open Access Journals (Sweden)

    Hari Pada Seal

    2012-06-01

    Full Text Available This article describes a simple solvent extraction method for the extraction of colorants from the three morphotypes such as, (Morphotype-1 (M1, Morphotype-2 (M2, and Morphotype-3 (M3 of Annatto (Bixa orellana L. seeds, and their separation, vivid, and qualitative demonstration by thin-layer chromatography. Several solvent systems (hexane, chloroform, acetone, ethanol, and a mixed-solvent having composition of CHCl3/C2H5OH/CH3COOH (80:2:1 were applied for extraction of colored components. It was observed that a large portion of colorants was extracted by chloroform. Its effluent was deep brick red in color and transparent. Furthermore, various carrier solvent systems (Benzene-Ethyl acetate were used to separate the components from the extracts. Carrier solvent system with the ratio of 7:3 was found as superior solvent for chloroform extracts. Three colored-spots were observed for all morphotypes. Among them, the first one was yellow colored having very low polarity and the second and third spots were both redbrick colored having medium and higher polarity respectively. In addition, for M1 no colorless-spot was observed in low and medium polar systems, revealing that the amount of wax and gum were minimum in the extract and superior morphotype among the three.

  1. Thin layer coulometry with ionophore based ion-selective membranes.

    Science.gov (United States)

    Grygolowicz-Pawlak, Ewa; Bakker, Eric

    2010-06-01

    We are demonstrating here for the first time a thin layer coulometric detection mode for ionophore based liquid ion-selective membranes. Coulometry promises to achieve the design of robust, calibration free sensors that are especially attractive for applications where recalibration in situ is difficult or undesirable. This readout principle is here achieved with porous polypropylene tubing doped with the membrane material and which contains a chlorinated silver wire in the inner compartment, together with the fluidically delivered sample solution. The membrane material consists of the lipophilic plasticizer dodecyl 2-nitrophenyl ether, the lipophilic electrolyte ETH 500, and the calcium ionophore ETH 5234. Importantly and in contrast to earlier work on voltammetric liquid membrane electrodes, the membrane also contains a cation-exchanger salt, KTFPB. This renders the membrane permselective and allows one to observe open circuit potentiometric responses for the device, which is confirmed to follow the expected Nernstian equation. Moreover, as the same cationic species is now potential determining at both interfaces of the membrane, it is possible to use rapidly diffusing and/or thin membrane systems where transport processes at the inner and outer interface of the membrane do not perturb each other or the overall composition of the membrane. The tubing is immersed in an electrolyte solution where the counter and working electrode are placed, and the potentials are applied relative to the measured open circuit potentials. Exhaustive current decays are observed in the range of 10 to 100 muM calcium chloride. The observed charge, calculated as integrated currents, is linearly dependent on concentration and forms the basis for the coulometric readout of ion-selective membrane electrodes.

  2. Determination of 4-Chloroindole-3-Acetic Acid Methyl Ester in Lathyrus Vicia and Pisum by Gas Chromatography - Mass Spectrometry

    DEFF Research Database (Denmark)

    Engvild, Kjeld Christensen; Egsgaard, Helge; Larsen, Elfinn

    1980-01-01

    4-Chloroindole-3-acetic acid methyl ester was identified unequivocally in Lathyrus latifolius L., Vicia faba L. and Pisum sativum L. by thin layer chromatography, gas chromatography and mass spectrometry. The gas chromatographic system was able to separate underivatized chloroindole-3-acetic acid...... methyl ester isomers. The quantitative determination of 4-chloroindole-3-acetic acid methyl ester in immature seeds of these three species was performed by gas chromatography – mass spectrometry using deuterium labelled 4-chloro-indole-3-acetic acid methyl ester as an internal standard. P. sativum...

  3. Antidiarrheal potential of standardized extract of Rhododendron arboreum Smith flowers in experimental animals

    OpenAIRE

    Neeraj Verma; Singh, Anil P.; Amresh Gupta; Sahu, P.K.; Ch V Rao

    2011-01-01

    Objective : To investigate standardized ethyl acetate fraction of Rhododendron arboreum (EFRA) flowers for antidiarrheal activity in experimental animals. Materials and Methods : A simple sensitive high performance thin layer chromatography (HPTLC) method was used for the determination of hyperin in EFRA. The standardized fraction was investigated for castor oil, magnesium sulfate-induced diarrhea, measurement of gastrointestinal transit using charcoal and castor oil-induced enteropooling...

  4. Qualitative detection of some electron donor drugs on thin-layer ...

    African Journals Online (AJOL)

    Qualitative detection of some electron donor drugs on thin-layer plates: chloranilic acid as ... A chromatographic procedure for the qualitative detection of ... coloration of the different complexes as a basis, it was possible to gain some insight ...

  5. Thin layers and species-specific characterization of the phytoplankton community in Monterey Bay, California, USA

    Science.gov (United States)

    Rines, J. E. B.; McFarland, M. N.; Donaghay, P. L.; Sullivan, J. M.

    2010-01-01

    During the summers of 2005 and 2006, experiments designed to understand the properties of densely concentrated, thin layers of plankton and the processes governing their dynamics were conducted in Monterey Bay, California, USA. Our goal was to elucidate the role that species-specific properties of phytoplankton play in thin layer dynamics. Using adaptive sampling, we collected water samples from inside and outside bio-optical features of the water column. Characterization of the phytoplankton was compiled from live and preserved samples, and analyzed within a framework of physical, optical, chemical and acoustical data. In both years, Monterey Bay was home to an extraordinarily diverse assemblage of phytoplankton and other protists. Bioluminescent dinoflagellates, and Harmful Algal Bloom (HAB) taxa were common. In 2005, community assemblages were widespread, thus advection of water through the experimental mooring array did not result in floristic changes. In 2006 phytoplankton were very patchy in horizontal distribution, and advection of water through the array was at times accompanied by dramatic shifts in community composition. Individual taxa often exhibited disparate patterns of vertical distribution, with some found throughout the water column, whereas others were restricted to narrow depth intervals. Thin layers were observed in both years. In 2005, the dinoflagellate Akashiwo sanguinea formed intense thin layers near the pycnocline at night, and migrated to near surface waters at dawn. In 2006, layer composition was more complex, and related to the water mass present at the time of sampling. Optically detected thin layers of phytoplankton can be studied from the perspective of the impact their high biomass has on both ecological processes, and ocean optics. But thin layers can also be studied from the species-specific perspective of each organism, its role within the thin layer habitat, and the impact that life within a thin layer has on its life history

  6. Amplitude various angles (AVA) phenomena in thin layer reservoir: Case study of various reservoirs

    Energy Technology Data Exchange (ETDEWEB)

    Nurhandoko, Bagus Endar B., E-mail: bagusnur@bdg.centrin.net.id, E-mail: bagusnur@rock-fluid.com [Wave Inversion and Subsurface Fluid Imaging Research Laboratory (WISFIR), Basic Science Center A 4" t" hfloor, Physics Dept., FMIPA, Institut Teknologi Bandung (Indonesia); Rock Fluid Imaging Lab., Bandung (Indonesia); Susilowati, E-mail: bagusnur@bdg.centrin.net.id, E-mail: bagusnur@rock-fluid.com [Rock Fluid Imaging Lab., Bandung (Indonesia)

    2015-04-16

    Amplitude various offset is widely used in petroleum exploration as well as in petroleum development field. Generally, phenomenon of amplitude in various angles assumes reservoir’s layer is quite thick. It also means that the wave is assumed as a very high frequency. But, in natural condition, the seismic wave is band limited and has quite low frequency. Therefore, topic about amplitude various angles in thin layer reservoir as well as low frequency assumption is important to be considered. Thin layer reservoir means the thickness of reservoir is about or less than quarter of wavelength. In this paper, I studied about the reflection phenomena in elastic wave which considering interference from thin layer reservoir and transmission wave. I applied Zoeppritz equation for modeling reflected wave of top reservoir, reflected wave of bottom reservoir, and also transmission elastic wave of reservoir. Results show that the phenomena of AVA in thin layer reservoir are frequency dependent. Thin layer reservoir causes interference between reflected wave of top reservoir and reflected wave of bottom reservoir. These phenomena are frequently neglected, however, in real practices. Even though, the impact of inattention in interference phenomena caused by thin layer in AVA may cause inaccurate reservoir characterization. The relation between classes of AVA reservoir and reservoir’s character are different when effect of ones in thin reservoir and ones in thick reservoir are compared. In this paper, I present some AVA phenomena including its cross plot in various thin reservoir types based on some rock physics data of Indonesia.

  7. Thin-layer thermal insulation coatings based on high-filled spheroplastics with polyorganosiloxane binder

    Science.gov (United States)

    Chukhlanov, V. Yu; Selivanov, O. G.; Trifonova, T. A.; Ilina, M. E.; Chukhlanova, N. V.

    2017-10-01

    Thermal insulation coatings, based on polyorganosiloxane as a binder and hollow glass microspheres, have been studied in this research. The developed materials are widely applied in various branches of science and engineering basically in construction. Components interaction processes are comprehensively studied. Spraying production methods of thin layer thermal insulation coatings have been researched. Ideal technological parameters for polyorganosiloxane coatings hardening depending on components ratio, ambient temperature, solvent and curative concentration have been determined. Stress related characteristics of constructional energy saving materials containing polyorganosiloxane have been researched. Components structure and ratio concerning compound extension strength properties have been revealed. Substantiation of Danneberg model application for the strength characteristics enhancing, when hollow microspheres are introduced, has been suggested. Thermal properties of coating thermal insulation have been studied. To research these characteristics standard methods applying devices IT-S-400 and IT-λ-400 have been chosen. Filler concentration increase was stated to decrease the composition heat conductivity coefficient and to the reduction of temperature dependence of this index. The authors suggested to employ the developed thermal insulation materials for construction and power engineering facilities operating under high temperature and other unfavorable environment.

  8. Novel thin layer flow-cell screen-printed graphene electrode for enzymatic sensors.

    Science.gov (United States)

    Kanso, Hussein; González García, María Begoña; Llano, Laura Fernández; Ma, Su; Ludwig, Roland; Fanjul Bolado, Pablo; Santos, David Hernández

    2017-07-15

    A new Screen-printed electrodes (SPE) integrated in one channel flow-cell was developed. The one channel flow-cell is attached and directly changeable with electrode. In the new flow-cell the injection is done through an "in-line luer injection port" which can be less aggressive than wall-jet flow cell for a biological recognition element immobilized on the surface of the electrode. The sample volume can be easily controlled by the operator through a syringe. In this novel thin layer flow-cell screen-printed electrodes, the working electrode was modified with graphene materials, and an enhancement of electroactive area to 388% over a standard electrode was found. This new configuration was applied to study the entrapped cellobiose dehydrogenase from the ascomycete Corynascus thermophilus (CtCDH) in a photocrosslinkable PVA-based polymer. The calibration curve of lactose using optimized parameters shows a wide linear measurement ranges between 0.25 and 5mM. A good operational stability of the CtCDH-PVA-modified graphene electrode is obtained, which keeps the same initial activity during 8h and exhibits a good storage stability with a decrease of only 9% in analytical response after 3 months storage at 4◦C. Copyright © 2016. Published by Elsevier B.V.

  9. Thin-layer solar drying characteristics of rough rice under natural convection

    Energy Technology Data Exchange (ETDEWEB)

    Basunia, M.A. [Bangladesh Agricultural University, Mymensingh (Bangladesh). Department of Farm Power and Machinery; Abe, T. [Ehime University, Matsuyama (Japan). Department of Biomechanical Systems, Laboratory of Agricultural Process Engineering

    2001-07-01

    Thin-layer solar drying experiments were conducted at Matsuyama, Japan, with medium grain rough rice. The range of average drying air temperature was 22.3 - 34.9 deg C, and the relative humidities were between 34.5 per cent and 57.9 per cent. The initial moisture contents were in the range of 37.07 - 37.69 per cent dry-basis. A mixed-mode natural convection solar grain dryer was used for this experiment. The data of sample weight and dry- and wet-bulb temperatures of the drying air were recorded continuously from morning to evening for each test. The drying data were then fitted to the Page model, based on the ratios of the differences between the initial and final moisture contents and the equilibrium moisture content (EMC). The model gave a good fit for the moisture content with an average standard error of 0.00387 dry-basis. Both the drying parameters N and K are linear functions of temperature and relative humidity. This single-layer drying equation can be used for the simulation of deep bed drying of rough rice in mixed-mode type natural convection solar dryers. (author)

  10. Development and Validation of Thin Layer Chromatograpy-Densitometry Method for Determinationa and Quantification of Sinthetic Red Coloring Agent in Sauce Sambel Sachet

    OpenAIRE

    Armin, Fithriani; Revira, Bita; Adnan, Adek Zamrud

    2015-01-01

    Chili sauce sachet A, B and C containing synthetic red coloring agent were taken from three fast food premises in Padang. Synthetic red coloring agent were a food additives used by food manufacturers to enhance color of food products. The use of food coloring agent in Indonesia were regulated in The Rule of Head of the Supervisory Food Board of the Republic of Indonesia Number 37 Year 2013 about the Limit Use of Food Coloring Agent. Thin-layer chromatography (TLC) -densitometry was a pre...

  11. Chromatography

    Science.gov (United States)

    ... that are bonded together. For example, water is a chemical bond of oxygen and hydrogen. Proteins are another type of chemical compound. There are different kinds of chromatography. These include gas, high pressure liquid, or ion ...

  12. Separation techniques: Chromatography

    Science.gov (United States)

    Coskun, Ozlem

    2016-01-01

    Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

  13. Surface Morphology of Fe(III-Porphyrin Thin Layers as Characterized by Atomic Force Microscopy

    Directory of Open Access Journals (Sweden)

    Utari Utari

    2016-12-01

    Full Text Available Surface morphology of Fe(III–porphyrin thin layers was studied using atomic force microscopy. The thin layer samples used in these experiments were deposited by spin coating methods on indium–tin-oxide substrates at room temperature under atmospheric conditions. Variations of thin layer of Fe(III-porphyrin were done by modifying the rotational speed and the concentration of the solution. The experimental results demonstrated that the Fe(III–porphyrin layers were observed as discrete nanomolecular islands. Both the number of nano-islands and thickness of the layer increased significantly with increasing concentration. A layer thickness of 15 nm was obtained for low concentrations of 0.00153 M and become 25 nm for dense concentrations of 0.153 M. Conversely, the higher number of islands were deposited on the surface of the substrate at a lower rotational speed.

  14. Thin layer microcolony culture associated with PCR for early identification of Mycobacterium bovis

    Directory of Open Access Journals (Sweden)

    Tatiana Reis do Rosário

    2014-01-01

    Full Text Available The initial growth of mycobacteria from 49 samples of cattle and buffalo organs collected in commercial slaughterhouses was compared between modified Middlebrook 7H11 thin layer microcolony culture and Stonebrink medium used in the isolation of Mycobacterium bovis. Aliquots were decontaminated by Petroff's method, processed and cultured in both media. The identity of the acid-fast bacilli stained by Ziehl-Neelsen was confirmed by PCR. Optical microscopy showed that results of the early observation of Mycobacterium bovis colonies in thin layer culture were similar to those obtained in macroscopic observation of the colonies in Stonebrink medium. However, early observation of the colonies enabled early confirmation by PCR, given the shorter time to the visualization of colonies when thin layer culture was used (between the 12nd and 25th day of culture.

  15. A model for thin layer formation by delayed particle settling at sharp density gradients

    Science.gov (United States)

    Prairie, Jennifer C.; White, Brian L.

    2017-02-01

    Thin layers - regions where plankton or particles accumulate vertically on scales of a few meters or less - are common in coastal waters, and have important implications for both trophic dynamics and carbon cycling. These features can form by a variety of biological and physical mechanisms, including localized growth, shear-thinning, and directed swimming. An additional mechanism may result in the formation of thin layers of marine aggregates, which have been shown to decrease their settling velocity when passing through sharp density gradients, a behavior termed delayed settling. Here, we apply a simple vertical advection-diffusion model to predict the properties of aggregate thin layers formed by this process. We assume a constant vertical flux of particles from the surface, which is parameterized by observations from laboratory experiments with marine aggregates. The formation, maintenance, and shape of the layers are described in relation to non-dimensional numbers that depend on environmental conditions and particle settling properties. In particular, model results demonstrate layer intensity and sharpness both increase with higher Péclet number (Pe), that is, under conditions with weaker mixing relative to layer formation. Similarly, more intense and sharper layers are found when the delayed settling behavior of aggregates is characterized by a lower velocity minimum. The model also predicts layers that are vertically asymmetric and highly "peaky" when compared with a Gaussian distribution, features often seen in thin layers in natural environments. Lastly, by comparing model predictions with observations of thin layers in the field, we are able to gain some insight into the applicability of delayed settling as a thin layer formation mechanism in different environmental conditions.

  16. Development of a quantitative high-performance thin-layer chromatographic method for sucralose in sewage effluent, surface water, and drinking water.

    Science.gov (United States)

    Morlock, Gertrud E; Schuele, Leonard; Grashorn, Sebastian

    2011-05-13

    Sucralose, a persistent chlorinated substance used as sweetener, can already be found in waste water, and various countries focused on the release of sucralose into the aquatic environment. A quantitative high-performance thin-layer chromatography (HPTLC) method, which is orthogonal to existing methods, was developed to analyze sucralose in water. After sample preparation, separation of up to 17 samples was performed in parallel on a HPTLC plate silica gel 60 F(254) with a mixture of isopropyl acetate, methanol and water (15:3:1, v/v/v) within 15 min. Due to the weak native UV absorption of sucralose (≤200 nm), various post-chromatographic derivatization reactions were compared to selectively detect sucralose in effluent and surface water matrices. Thereby p-aminobenzoic acid reagent was discovered as a new derivatization reagent for sucralose. Compared to the latter and to β-naphthol, derivatization with aniline diphenylamine o-phosphoric acid reagent was slightly preferred and densitometry was performed by absorbance measurement at 400 nm. The limit of quantification (LOQ) of sucralose in drinking and surface water was calculated to be 100 ng/L for a given recovery rate of 80% and the extraction of a 0.5 L water sample. The sucralose content determined in four water samples obtained during an interlaboratory trial in 2008 was in good agreement to the mean laboratory values of that trial. According to the t-test, which compares the results with the target value, the means obtained by HPTLC were not significantly different from the respective means of six laboratories, analyzed by HPLC-MS/MS or HPLC-TOF-MS with the use of mostly isotopically labeled standards. The good accuracy and high sample throughput capacity proved HPTLC as a well suited method regarding quantification of sucralose in various aqueous matrices. Copyright © 2010 Elsevier B.V. All rights reserved.

  17. Development and Validation Of Thin Layer Chromatograpy-Densitometry Method for Determinationa and Quantification of Sinthetic Red Coloring Agent in Sauce Sambel Sachet

    Directory of Open Access Journals (Sweden)

    Fithriani Armin

    2015-12-01

    Full Text Available Chili sauce sachet A, B and C containing synthetic red coloring agent  were taken from three fast food premises in Padang. Synthetic red coloring agent  were a food additives used by food manufacturers to enhance color of food products. The use of food coloring agent in Indonesia were regulated   in The Rule of Head of the Supervisory Food Board of the Republic of Indonesia Number 37 Year 2013 about the Limit Use of Food Coloring Agent. Thin-layer chromatography (TLC -densitometry was  a precision method for the analysis of food additives. Development and validation of TLC method for chromatographic separation used GF254 silica plate eluted with a mixture of ethanol: butanol: distilled water (4: 5: 5 and spots were detected visually. A red spots on the sample B was identified as Ponceau 4R with Rf value of 0.76. It was then followed by quantitative analysis using densitometry. The linearity of the method  was found in the range of 2-10μg/ml with a correlation coefficient of 0.994. Precision intra-day and inter-day relative standard deviation was shown from 1.11% and 2.69% respectively. Accuracy of the method was shown on the percentage of recovery of the 3 different concentrations of solution which gave the average percentage of 108.17%. Limit of detection and limit quantitation was 0.8306μg/ml and 2.7687μg/ml.  The concentration of Ponceau 4R in the sample B was 11.9520mg/kg of material. This value was not exceeded the  maximum concentration of food coloring agent as stated in the rule which should not be above 70mg/kg of material.

  18. The Mobile Phase Motion in Ascending Micellar Thin-Layer Chromatography with Normal-Phase Plates

    NARCIS (Netherlands)

    Boichenko, Alexander P.; Makhno, Iryna V.; Renkevich, Anton Yu.; Loginova, Lidia P.

    2011-01-01

    The physical chemical characteristics (surface tension and viscosity) of micellar mobile phases based on the cationic surfactant cetylpiridinium chloride and additives of alcohols (ethanol, 1-propanol, 1-butanol, 1-pentanol) have been obtained in this work. The effect of mobile phase properties on

  19. Determination of sucralose in soft drinks by high-performance thin-layer chromatography: interlaboratory study.

    Science.gov (United States)

    Stroka, Joerg; Doncheva, Ivanka; Spangenberg, Bernd

    2009-01-01

    An interlaboratory comparison was carried out to evaluate the effectiveness of a method based on HPTLC in which reagent-free derivatization is followed by UV/fluorescence detection. The method was tested for the determination of sucralose (C12H19C13O8; (2R,3R,4R,5S,6R)-2-[(2R,3S,4S,5S)-2,5-bis(chloromethyl)-3,4-dihydroxyoxolan-2-yl]oxy-5-chloro-6-hydroxymethyl)oxane-3, 4-diol; CAS Registry No. 56038-13-2) in carbonated and still beverages at the proposed European regulatory limits. For still beverages, a portion of the sample was diluted with methanol-water. For carbonated beverages, a portion of the sample was degassed in an ultrasonic bath before dilution. Turbid beverages were filtered after dilution through an HPLC syringe filter. The separation of sucralose was performed by direct application on amino-bonded (NH2) silica gel HPTLC plates (no cleanup needed) with the mobile phase acetonitrile-water. Sucralose was determined after reagent-free derivatization at 190 degrees C; it was quantified by measurements of both UV absorption and fluorescence. The samples, both spiked and containing sucralose, were sent to 14 laboratories in five different countries. Test portions of a sample found to contain no sucralose were spiked at levels of 30.5, 100.7, and 299 mg/L. Recoveries ranged from 104.3 to 124.6% and averaged 112% for determination by UV detection; recoveries ranged from 98.4 to 101.3% and averaged 99.9% for determination by fluorescence detection. On the basis of the results for spiked samples (blind duplicates at three levels), as well as sucralose-containing samples (blind duplicates at three levels and one split level), the values for the RSDr ranged from 10.3 to 31.4% for determinations by UV detection and from 8.9 to 15.9% for determinations by fluorescence detection. The values for the RSDR values ranged from 13.5 to 31.4% for determinations by UV detection and from 8.9 to 20.7% for determinations by fluorescence detection.

  20. Quantitative determination of ruscogenin in Ruscus species by densitometric thin-layer chromatography.

    Science.gov (United States)

    Nikolov, S; Joneidi, M; Panova, D

    1976-01-01

    A densitometric t.l.c. method of quantitative determination of ruscogenin was elaborated. After separation with the aid of t.l.c., the colourless ruscogenin spots were located with the aid of a p-dimethyl-aminobenzaldehyde solution and were submitted to densitometry. It was found that under the selected conditions a linear dependence exists between the betaI% value and lgC within the range of 0.5--10 mug ruscogenin. The determination of ruscogenin is done in the presence of the remaining components of the sample. The method is free of any systematic error. The method was applied in the determination of the ruscogenin content of the above-ground and underground part of Ruscus aculeatus and R. hypoglossum, extracts of the same plants, and capsules with further to the R. aculeatus extract also contained bioflavonoids. It was found that the content of ruscogenin in the underground and the above-ground parts of R. hypoglossum is 0.14 and 0.10%, respectively, while for R. aculeatus the respective values are 0.12 and 0.08%. The extract contains 1.6% ruscogenin, and the capsules 0.09 mg each.

  1. Evaluation of alternative rapid thin layer chromatography systems for quality control of technetium-99m radiopharmaceuticals.

    Science.gov (United States)

    Mang'era, Kennedy; Wong, Derek; Douglas, David; Franz, Kellie; Biru, Taddese

    2014-04-01

    Whatman 3MM™ and Tec-Control™ systems were evaluated as ITLC-SG alternatives for 99mTc-radiopharmaceuticals. They compare well in accuracy and reproducibility, and are faster and more convenient than ITLC-SG. Tec-Control™ radiochemical purity values for 99mTc-sestamibi were more conservative than ITLC-SG. Full solvent migration was not reproduced for 99mTc-tetrofosmin in Tec-Control™, and for this Whatman 3MM™ is preferred. Developing times were 10-15 min, 7-9 min and ~1min for ITLC-SG, Whatman 3MM™ and Tec-Control™, respectively. Overall, Tec-Control™ strips are preferred due to speed and ease of use. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. Reversed-phase thin-layer chromatography of homologs of Antimycin-A and related derivatives

    Science.gov (United States)

    Abidi, Sharon L.

    1989-01-01

    Using a reversed-phase high-performance liquid chromatographic (HPLC) technique, a mixture of antimycins A was separated into eight hitherto unreported subcomponents, Ala, Alb, A2a, A2b, A3a, A3b, A4a, and A4b. Although a base-line resolution of the known four major antimycins Al, A2, A3, and A4 was readily achieved with mobile phases containing acetate buffers, the separation of the new antibiotic subcomponents was highly sensitive to variation in mobile phase conditions. The type and composition of organic modifiers, the nature of buffer salts, and the concentration of added electrolytes had profound effects on capacity factors, separation factors, and peak resolution values. Of the numerous chromatographic systems examined, a mobile phase consisting of methanol-water (70:30) and 0.005 M tetrabutylammonium phosphate at pH 3.0 yielded the most satisfactory results for the separation of the subcomponents. Reversed-phase gradient HPLC separation of the dansylated or methylated antibiotic compounds produced superior chromatographic characteristics and the presence of added electrolytes was not a critical factor for achieving separation. Differences in the chromatographic outcome between homologous and structural isomers were interpretated based on a differential solvophobic interaction rationale. Preparative reversed-phase HPLC under optimal conditions enabled isolation of pure samples of the methylated antimycin subcomponents for use in structural studies.

  3. Assessment of doses caused by electrons in thin layers of tissue-equivalent materials, using MCNP.

    Science.gov (United States)

    Heide, Bernd

    2013-10-01

    Absorbed doses caused by electron irradiation were calculated with Monte Carlo N-Particle transport code (MCNP) for thin layers of tissue-equivalent materials. The layers were so thin that the calculation of energy deposition was on the border of the scope of MCNP. Therefore, in this article application of three different methods of calculation of energy deposition is discussed. This was done by means of two scenarios: in the first one, electrons were emitted from the centre of a sphere of water and also recorded in that sphere; and in the second, an irradiation with the PTB Secondary Standard BSS2 was modelled, where electrons were emitted from an (90)Sr/(90)Y area source and recorded inside a cuboid phantom made of tissue-equivalent material. The speed and accuracy of the different methods were of interest. While a significant difference in accuracy was visible for one method in the first scenario, the difference in accuracy of the three methods was insignificant for the second one. Considerable differences in speed were found for both scenarios. In order to demonstrate the need for calculating the dose in thin small zones, a third scenario was constructed and simulated as well. The third scenario was nearly equal to the second one, but a pike of lead was assumed to be inside the phantom in addition. A dose enhancement (caused by the pike of lead) of ∼113 % was recorded for a thin hollow cylinder at a depth of 0.007 cm, which the basal-skin layer is referred to in particular. Dose enhancements between 68 and 88 % were found for a slab with a radius of 0.09 cm for all depths. All dose enhancements were hardly noticeable for a slab with a cross-sectional area of 1 cm(2), which is usually applied to operational radiation protection.

  4. Bergenin determination in different extracts by high-performance thin-layer chromatographic densitometry

    Science.gov (United States)

    Khan, Masood Shah; Khan, Washim; Ahmad, Wasim; Singh, Mhaveer; Ahmad, Sayeed

    2015-01-01

    Aim: Bergenin is an active secondary metabolite, found in Bergenia ligulata, family Saxifragaceae, which is an important medicinal plant used in the traditional system of medicine. It is distributed throughout the South and East Asia and some European countries, usually growing on high altitude in the Himalayan region and known as Pashanbhed (meaning “to break the stone”). The rhizome of B. ligulata has been used since long time in different traditional formulations of kidney and liver disorders. Due to its exhaustive use in the traditional system, it is commonly adulterated with the rhizome of other plants which do not contain its chemical marker bergenin. Hence, we developed high-performance thin-layer chromatographic (HPTLC) method for quantification of bergenin in B. ligulata which can be used for its quality control. Materials and Methods: A sensitive HPTLC method has been developed for the estimation of bergenin in different extracts of B. ligulata and its traditional formulations. Precoated HPTLC silica gel plates were used as stationary phase, and chloroform: methanol: acetic acid (8:1:1, v/v/v) was used as mobile phase. Results: The Rf value of bergenin was found to be 0.28 ± 0.03. Detection and quantification were performed by densitometry at 276 nm. The calibration plot was linear in the range of 200–5000 ng of bergenin with the correlation coefficient of (r2) 0.999, which confirms good linearity. The content of bergenin in methanolic and acetone extracts was found to be 5.51 ± 0.14 and 5.76 ± 0.16, respectively. Conclusion: The method can be applied for quality control and standardization of B. ligulata and its traditional formulations as well as for checking the presence of adulterants. PMID:26681881

  5. A mass transfer model of ethanol emission from thin layers of corn silage

    Science.gov (United States)

    A mass transfer model of ethanol emission from thin layers of corn silage was developed and validated. The model was developed based on data from wind tunnel experiments conducted at different temperatures and air velocities. Multiple regression analysis was used to derive an equation that related t...

  6. Moisture removal characteristics of thin layer rough rice under sequenced infrared radiation heating and cooling

    Science.gov (United States)

    Rice drying with infrared (IR) radiation has been investigated during recent years and showed promising potential with improved quality and energy efficiency. The objective of this study was to further investigate the moisture removal characteristics of thin layer rough rice heated by IR and cooled ...

  7. Bearing Capacity of Footings on Thin Layer of Sand on Soft Cohesive Soil

    DEFF Research Database (Denmark)

    Philipsen, J.; Sørensen, Carsten S.

    2004-01-01

    This paper contains the results of some numerical calculations performed with the aim to determine the bearing capacities of footings placed on a thin layer of sand underlain by soft cohesive soil. During the last 30-35 years different analytical and empirical calculation methods for this situation...... prepared model tests made in laboratories....

  8. A thin-layer solution of the flow about a prolate spheroid

    Science.gov (United States)

    Panaras, A. G.; Steger, J. L.

    1988-01-01

    Computational results are presented for the transitional or turbulent flow about a prolate spheroid, at alpha = 10 deg or 30 deg, correspondingly, using an implicit, approximately factored, partially flux-split algorithm, based on the thin-layer equations. The computed flow field is in good agreement with available experimental data.

  9. A thin layer fiber-coupled luminescence dosimeter based on Al2O3:C

    DEFF Research Database (Denmark)

    Klein, F.A.; Greilich, Steffen; Andersen, Claus Erik

    2011-01-01

    In this paper we present a fiber-coupled luminescent Al2O3:C dosimeter probe with high spatial resolution (0.1 mm). It is based on thin layers of Al2O3:C crystal powder and a UV-cured acrylate monomer composition. The fabrication of the thin layers is described in detail. No influence of the intr......In this paper we present a fiber-coupled luminescent Al2O3:C dosimeter probe with high spatial resolution (0.1 mm). It is based on thin layers of Al2O3:C crystal powder and a UV-cured acrylate monomer composition. The fabrication of the thin layers is described in detail. No influence...... of the introduced polymer host matrix on the dosimetric properties was observed. Depth-dose measurements with the new detectors in a 142.66 MeV proton and 270.55 MeV/u carbon ion beam are presented as example applications. We used an RL protocol with saturated crystals allowing for time-effective measurements...... of the protons measured with this new detector deviated by less than 1% from the reference value. For both ion types, the stem effect contributed less than 0.8% of the RL signal....

  10. Ethanol as Internal Standard for Quantitative Determination of Volatile Compounds in Spirit Drinks by Gas Chromatography

    CERN Document Server

    Charapitsa, Siarhei V; Kulevich, Nikita V; Makoed, Nicolai M; Mazanik, Arkadzi L; Sytova, Svetlana N

    2012-01-01

    The new methodical approach of using ethanol as internal standard in gas chromatographic analysis of volatile compounds in spirit drinks in daily practice of testing laboratories is proposed. This method provides determination of volatile compounds concentrations in spirit drinks directly expressed in milligrams per liter (mg/L) of absolute alcohol according to official methods without measuring of alcohol strength of analyzed sample. The experimental demonstration of this method for determination of volatile compounds in spirit drinks by gas chromatography is described. Its validation was carried out by comparison with experimental results obtained by internal standard method and external standard method.

  11. Physico-chemical standardization of Sitopaladi churna

    Science.gov (United States)

    Makhija, Inder Kumar; Shreedhara, Chandrashekara Shastry; Ram, Holavana Hally Nanjundaiah Setty Aswatha

    2012-01-01

    Background: Standardization of a compound Ayurvedic formulation is a critical and essential issue to be considered in assuring the therapeutic efficacy and safety and to rationalize their use in the health care. Sitopaladi churna is a reputed polyherbal formulation of Ayurveda. It is prescribed for the treatment of pleurodynia, intercostal neuralgia, cold, cough associated with bronchitis, pneumonia, tuberculosis, viral respiratory infection, and in pharyngeal and chest congestion. Objective: The present study aimed at physico-chemical standardization of in-house and two marketed brands of Sitopaladi churna. Materials and Methods: In our investigation, in-house churna and two commercial brands of Sitopaladi churna were standardized based on powder microscopy, physico-chemical evaluations, thin layer chromatography (TLC) and high performance thin layer chromatography (HPTLC) finger printing as per standard procedures. Results: The set parameters were sufficient to evaluate the churna based on various physico-chemical parameters. Conclusion: The data evolved can be adopted for laying down the standards for the manufacturing units of Sitopaladi churna. PMID:23284216

  12. Mathematical modelling of the thin layer solar drying of banana, mango and cassava

    Energy Technology Data Exchange (ETDEWEB)

    Koua, Kamenan Blaise; Fassinou, Wanignon Ferdinand; Toure, Siaka [Laboratoire d' Energie Solaire, Universite de Cocody- Abidjan, 22 BP 582 Abidjan 22 (Ivory Coast); Gbaha, Prosper [Laboratoire d' Energie Nouvelle et Renouvelable, Institut National Polytechnique, Felix HOUPHOUET - BOIGNY de Yamoussoukro (Ivory Coast)

    2009-10-15

    The main objectives of this paper are firstly to investigate the behaviour of the thin layer drying of plantain banana, mango and cassava experimentally in a direct solar dryer and secondly to perform mathematical modelling by using thin layer drying models encountered in literature. The variation of the moisture content of the products studied and principal drying parameters are analysed. Seven statistical models, which are empirical or semi-empirical, are tested to validate the experimental data. A non-linear regression analysis using a statistical computer program is used to evaluate the constants of the models. The Henderson and Pabis drying model is found to be the most suitable for describing the solar drying curves of plantain banana, mango and cassava. The drying data of these products have been analysed to obtain the values of the effective diffusivity during the falling drying rate phase. (author)

  13. Mathematical modelling of a thin layer drying of apricots in a solar energized rotary dryer

    Energy Technology Data Exchange (ETDEWEB)

    Akpinar, E.K.; Yildiz, C. [Firat Univ., Elazig (Turkey). Dept. of Mechanical Engineering; Sarsilmaz, C. [Firat Univ., Elazig (Turkey). Dept. of Mechanical Education

    2004-07-01

    In this paper we present a mathematical modelling of a thin layer forced solar drying of apricots. An indirect forced convection solar dryer consisting of a solar heater and a rotary column cylindrical drying (RCCD) cabinet was used in the experiments. Air heated by the solar air heater was forced through the apricots by an electrical fan. Moreover, the natural sun drying experiments were conducted for the comparison at the same time. Fourteen different thin layer mathematical drying models were compared according to their coefficients of determination (r,{chi}{sup 2}, RMSE) to estimate solar drying curves. The effects of the drying air temperature, velocity and the rotation speed of column on the drying model constants and coefficients were predicted by multiple regressions using a linear type model. (Author)

  14. On elastic waves in an thinly-layered laminated medium with stress couples under initial stress

    Directory of Open Access Journals (Sweden)

    P. Pal Roy

    1988-01-01

    Full Text Available The present work is concerned with a simple transformation rule in finding out the composite elastic coefficients of a thinly layered laminated medium whose bulk properties are strongly anisotropic with a microelastic bending rigidity. These elastic coefficients which were not known completely for a layered laminated structure, are obtained suitably in terms of initial stress components and Lame's constants λi, μi of initially isotropic solids. The explicit solutions of the dynamical equations for a prestressed thinly layered laminated medium under horizontal compression in a gravity field are derived. The results are discussed specifying the effects of hydrostatic, deviatoric and couple stresses upon the characteristic propagation velocities of shear and compression wave modes.

  15. Phonon and electron temperature and non-Fourier heat transport in thin layers

    Energy Technology Data Exchange (ETDEWEB)

    Carlomagno, I.; Cimmelli, V.A. [Department of Mathematics, Computer Science and Economics, University of Basilicata, Campus Macchia Romana, Viale dell' Ateneo Lucano 10, 85100 Potenza (Italy); Sellitto, A. [Department of Industrial Engineering, University of Salerno, Via Giovanni Paolo II, 132, 84084 Fisciano (Italy)

    2017-04-15

    We present a thermodynamic model of heat conductor which allows for different temperatures of phonons and electrons. This model is applied to calculate the steady-state radial temperature profile in a circular thin layer. The compatibility of the obtained temperature profiles with the second law of thermodynamics is investigated in view of the requirement of positive entropy production and of a nonlocal constitutive equation for the entropy flux.

  16. [Progress in thin layer CT scan technology in estimating skeletal age of sternal end of clavicle].

    Science.gov (United States)

    Wang, Ya-Hui; Wei, Hua; Ying, Chong-Liang; Wan, Lei; Zhu, Guang-You

    2013-04-01

    It is practical value for determination the teenagers whether the age is full of the legal responsibility age of 18 years old or not by estimating skeletal age of sternal end of clavicle. The traditional methods mainly based on X-ray radiography. However, sternal end of clavicle and adjacent lung, bronchus, sternum, rib, transverse process of thoracic vertebra are overlapped each other. As a result of overlapping, there will be obtained false negative or positive film reading results when according to X-ray observation of epiphyseal growth of sternal end of clavicle, which directly affect the scientificalness and accuracy of estimating of skeletal age. In recent years, the scholars at home and abroad have started to use thin layer CT scan technology to estimate skeletal age of the sternal end of clavicle. With the 2D and 3D CT recombination technology, the accuracy of the film reading distinctly improves by making the shape, size and position of epiphysis displayed clearly. This article reviews the application and research progress of thin layer CT scanning technology in estimating skeletal age of sternal end of clavicle at home and abroad, analyzes the superiority and value of thin layer CT scan technology, which applied to skeletal age of sternal end of clavicle.

  17. Separation of Caffeine from Beverages and Analysis Using Thin-Layer Chromatography and Gas Chromatography-Mass Spectrometry

    Science.gov (United States)

    Torres y Torres, Janelle L.; Hiley, Shauna L.; Lorimor, Steven P.; Rhoad, Jonathan S.; Caldwell, Benjamin D.; Zweerink, Gerald L.; Ducey, Michael

    2015-01-01

    The Characterization and Analysis of a Product (CAP) project is used to introduce first-semester general chemistry students to chemical instrumentation through the analysis of caffeine-containing beverage products. Some examples of these products have included coffee, tea, and energy drinks. Students perform at least three instrumental experiments…

  18. Planar chromatography for the hydrocarbon group type analysis of petroleum middle distillates and coal-derived products

    Energy Technology Data Exchange (ETDEWEB)

    Matt, Muriel; Gruber, Rene [Laboratoire de thermodynamique et d' analyses chimiques, Universite de Metz, Ile du Saulcy, UFR SciFA, 57045 cedex 1 Metz (France); Galvez, Eva; Cebolla, Vicente; Membrado, Luis; Vela, Jesus [Instituto de Carboquimica, CSIC, Miguel Luesma Castan 4, 50015 Zaragoza (Spain)

    2002-06-20

    Different methodologies, based on planar chromatography/detection with densitometry, have been used to analyse compound classes (also known as hydrocarbon group type (HGT)) in samples coming from petroleum and coal conversion. The main problem encountered to analyse these samples is the choice of standard: because of the high variability of the signal that is dependent of molecular structure, one pure hydrocarbon does not reflect the response of a mixture. However, a step based on thin layer chromatography at preparative scale has allowed the fractionation of sample to obtain its derived standards. After this, alkanes have been quantified by fluorescence in presence of berberine sulfate and aromatic compounds have been detected by UV after separation by high performance thin layer chromatography (HPTLC) at analytical scale.The feasibility of the planar chromatography has been tested. The quantitative results obtained for different samples are in agreement with those provided using well-established techniques in the petrochemical industry and the coal-derived product (CDP) analysis.

  19. [Isolation of toxic peptides from Amanita phalloides and their analysis using high-performance liquid chromatography].

    Science.gov (United States)

    Hampl, J

    1993-08-05

    The objective of the work is isolation of toxic peptides from Amanita phalloides--amatoxins (alfa-, beta-, gamma-amanitin) and phallotoxins (phalloidin, phallacidin, phallisin, phallisacin) by liquid chromatography on Sephadex LH-20 according to Yocum modification. Seven main toxins were isolated in centigram amounts. The purity of the toxins isolated was verified by the characteristics of their absorbance spectra, by thin layer chromatography (TLC) and high-performance liquid chromatography on reversed phase (RP-HPLC). The fraction of acid phallotoxins which appears homogenous in TLC and Sephadex LH-20 was separated into 5 substances (four of which are phallotoxins) by preparative RP-HPLC technique. The toxins isolated are sufficiently pure to be used as standards in HPLC.

  20. Investigation of thin layers deposited by two PVD techniques on high speed steel produced by powder metallurgy

    Science.gov (United States)

    Jakubéczyová, D.; Hvizdoš, P.; Selecká, M.

    2012-04-01

    This study was intended to investigate the properties and cutting performance with thin layers applied by two PVD techniques. PVD techniques ARC and LARC were used for the deposition of thin coatings onto cutting tools prepared by powder metallurgy. Advanced types of layers - monolayer AlTiCrN and nanocomposite type of nc-AlTiN/Si3N4 layer - were analyzed by standard techniques for surface status and quality assessment - roughness, hardness, layer thickness, chemical composition by GDOES, tribological properties at room and elevated temperature. Durability testing of the cutting tools was carried out according to the standard ISO 3685-1999. The nanocomposite nc-AlTiN/Si3N4 layer achieved lower roughness when compared to monolayer AlTiCrN which leads to the achievement of higher hardness and better layer quality. The HV0.5 hardness values were ∼26 GPa. The results showed a 2-3-times longer durability of the cutting tools in comparison with equivalent uncoated PM and traditional materials. The deposited coatings contributed to the improvement of their durability.

  1. Validated high-performance thin-layer chromatographic (HPTLC method for simultaneous determination of nadifloxacin, mometasone furoate, and miconazole nitrate cream using fractional factorial design

    Directory of Open Access Journals (Sweden)

    Kalpana G. Patel

    2016-07-01

    Full Text Available A high-performance thin-layer chromatographic method for simultaneous determination of nadifloxacin, mometasone furoate, and miconazole nitrate was developed and validated as per International Conference on Harmonization guidelines. High-performance thin-layer chromatographic separation was performed on aluminum plates precoated with silica gel 60F254 and methanol:ethyl acetate:toluene: acetonitrile:3M ammonium formate in water (1:2.5:6.0:0.3:0.2, % v/v as optimized mobile phase at detection wavelength of 224 nm. The retardation factor (Rf values for nadifloxacin, mometasone furoate, and miconazole nitrate were 0.23, 0.70, and 0.59, respectively. Percent recoveries in terms of accuracy for the marketed formulation were found to be 98.35–99.76%, 99.36–99.65%, and 99.16–100.25% for nadifloxacin, mometasone furoate, and miconazole nitrate, respectively. The pooled percent relative standard deviation for repeatability and intermediate precision studies was found to be < 2% for three target analytes. The effect of four independent variables, methanol content in total mobile phase, wavelength, chamber saturation time, and solvent front, was evaluated by fractional factorial design for robustness testing. Amongst all four factors, volume of methanol in mobile phase appeared to have a possibly significant effect on retention factor of miconazole nitrate compared with the other two drugs nadifloxacin and mometasone furoate, and therefore it was important to be carefully controlled. In summary, a novel, simple, accurate, reproducible, and robust high-performance thin-layer chromatographic method was developed, which would be of use in quality control of these cream formulations.

  2. Thin layer agar compared to BACTEC MGIT 960 for early detection of Mycobacterium tuberculosis.

    Science.gov (United States)

    Martin, Anandi; Fissette, Krista; Varaine, Francis; Portaels, Françoise; Palomino, Juan Carlos

    2009-07-01

    We compared the sensitivity and time to detection of growth of Mycobacterium tuberculosis in the thin layer agar (TLA) compared to BACTEC MGIT960. The average time for growth of M. tuberculosis in TLA and BACTEC MGIT960 was 10.6 and 9.6 days, respectively. The sensitivity of detection of M. tuberculosis was 97.3% on TLA and 97% on BACTEC MGIT960 for smear positive samples. TLA showed comparable results to BACTEC MGIT960 and could be an alternative method for low-income countries.

  3. Multiplicative effects model with internal standard in mobile phase for quantitative liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Song, Mi; Chen, Zeng-Ping; Chen, Yao; Jin, Jing-Wen

    2014-07-01

    Liquid chromatography-mass spectrometry assays suffer from signal instability caused by the gradual fouling of the ion source, vacuum instability, aging of the ion multiplier, etc. To address this issue, in this contribution, an internal standard was added into the mobile phase. The internal standard was therefore ionized and detected together with the analytes of interest by the mass spectrometer to ensure that variations in measurement conditions and/or instrument have similar effects on the signal contributions of both the analytes of interest and the internal standard. Subsequently, based on the unique strategy of adding internal standard in mobile phase, a multiplicative effects model was developed for quantitative LC-MS assays and tested on a proof of concept model system: the determination of amino acids in water by LC-MS. The experimental results demonstrated that the proposed method could efficiently mitigate the detrimental effects of continuous signal variation, and achieved quantitative results with average relative predictive error values in the range of 8.0-15.0%, which were much more accurate than the corresponding results of conventional internal standard method based on the peak height ratio and partial least squares method (their average relative predictive error values were as high as 66.3% and 64.8%, respectively). Therefore, it is expected that the proposed method can be developed and extended in quantitative LC-MS analysis of more complex systems. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Planar chromatography coupled with spectroscopic techniques.

    NARCIS (Netherlands)

    Somsen, G.W.; Wilson, I.D.; Morden, W.

    1995-01-01

    Recent progress in the combination of planar, or thin-layer chromatography (TLC) with a variety of modern spectroscopic techniques is reviewed. The utility of TLC for separation followed by mass spectrometry, with a variety of ionisation techniques, is illustrated with reference to a wide range of

  5. Modelling and experimental validation of thin layer indirect solar drying of mango slices

    Energy Technology Data Exchange (ETDEWEB)

    Dissa, A.O.; Bathiebo, J.; Kam, S.; Koulidiati, J. [Laboratoire de Physique et de Chimie de l' Environnement (LPCE), Unite de Formation et de Recherche en Sciences Exactes et Appliquee (UFR/SEA), Universite de Ouagadougou, Avenue Charles de Gaulle, BP 7021 Kadiogo (Burkina Faso); Savadogo, P.W. [Laboratoire Sol Eau Plante, Institut de l' Environnement et de Recherches Agricoles, 01 BP 476, Ouagadougou (Burkina Faso); Desmorieux, H. [Laboratoire d' Automatisme et de Genie des Procedes (LAGEP), UCBL1-CNRS UMR 5007-CPE Lyon, Bat.308G, 43 bd du 11 Nov. 1918 Villeurbanne, Universite Claude Bernard Lyon1, Lyon (France)

    2009-04-15

    The thin layer solar drying of mango slices of 8 mm thick was simulated and experimented using a solar dryer designed and constructed in laboratory. Under meteorological conditions of harvest period of mangoes, the results showed that 3 'typical days' of drying were necessary to reach the range of preservation water contents. During these 3 days of solar drying, 50%, 40% and 5% of unbound water were eliminated, respectively, at the first, second and the third day. The final water content obtained was about 16 {+-} 1.33% d.b. (13.79% w.b.). This final water content and the corresponding water activity (0.6 {+-} 0.02) were in accordance with previous work. The drying rates with correction for shrinkage and the critical water content were experimentally determined. The critical water content was close to 70% of the initial water content and the drying rates were reduced almost at 6% of their maximum value at night. The thin layer drying model made it possible to simulate suitably the solar drying kinetics of mango slices with a correlation coefficient of r{sup 2} = 0.990. This study thus contributed to the setting of solar drying time of mango and to the establishment of solar drying rates' curves of this fruit. (author)

  6. Desorption isotherms and mathematical modeling of thin layer drying kinetics of tomato

    Science.gov (United States)

    Belghith, Amira; Azzouz, Soufien; ElCafsi, Afif

    2016-03-01

    In recent years, there is an increased demand on the international market of dried fruits and vegetables with significant added value. Due to its important production, consumption and nutrient intake, drying of tomato has become a subject of extended and varied research works. The present work is focused on the drying behavior of thin-layer tomato and its mathematical modeling in order to optimize the drying processes. The moisture desorption isotherms of raw tomato were determined at four temperature levels namely 45, 50, 60 and 65 °C using the static gravimetric method. The experimental data obtained were modeled by five equations and the (GAB) model was found to be the best-describing these isotherms. The drying kinetics were experimentally investigated at 45, 55 and 65 °C and performed at air velocities of 0.5 and 2 m/s. In order to investigate the effect of the exchange surface on drying time, samples were dried into two different shapes: tomato halves and tomato quarters. The impact of various drying parameters was also studied (temperature, air velocity and air humidity). The drying curves showed only the preheating period and the falling drying rate period. In this study, attention was paid to the modeling of experimental thin-layer drying kinetics. The experimental results were fitted with four different models.

  7. EFFECT OF MECHANICAL CONDITIONING ON THIN-LAYER DRYING OF ENERGY SORGHUM (Sorghum bicolor (L.) Moench)

    Energy Technology Data Exchange (ETDEWEB)

    Ian J. Bonner; Kevin L. Kenney

    2012-10-01

    Cellulosic energy varieties of Sorghum bicolor (L.) Moench show promise as a bioenergy feedstock, however, high moisture content at the time of harvest results in unacceptable levels of degradation when stored in aerobic conditions. To safely store sorghum biomass for extended periods in baled format, the material must be dried to inhibit microbial growth. One possible solution is allowing the material to dry under natural in-field conditions. This study examines the differences in thin-layer drying rates of intact and conditioned sorghum under laboratory-controlled temperatures and relative humidity levels (20 degrees C and 30 degrees C from 40% to 85% relative humidity), and models experimental data using the Page’s Modified equation. The results demonstrate that conditioning drastically accelerates drying times. Relative humidity had a large impact on the time required to reach a safe storage moisture content for intact material (approximately 200 hours at 30 degrees C and 40% relative humidity and 400 hours at 30 degrees C and 70% relative humidity), but little to no impact on the thin-layer drying times of conditioned material (approximately 50 hours for all humidity levels < 70% at 30 degrees C). The drying equation parameters were influenced by temperature, relative humidity, initial moisture content, and material damage, allowing drying curves to be empirically predicted. The results of this study provide valuable information applicable to the agricultural community and to future research on drying simulation and management of energy sorghum.

  8. Investigation into the Thin Layer Drying Models of Nigerian Popcorn Varieties

    Directory of Open Access Journals (Sweden)

    Taiwo ADEMILUYI

    2008-12-01

    Full Text Available Drying kinetics of three popcorn varieties (Pin, Deep and Light yellow was investigated. The popcorn kernels initially conditioned to 25% moisture content were dried in a bench scale rotary drier to 14% moisture content at various air flow rates (0.83, 1.397, 2.79 m/s and temperatures (50oC, 60oC, 70oC and 80oC. Falling rate drying period was observed for the three popcorn varieties with Pin popcorn having the highest drying rate. Eight drying models were used to determine the thin layer drying kinetics. The Page equation, Two term model, Modified Page were found the best to describe the thin layer drying of Pin, Light yellow and Deep yellow popcorn, but the newly proposed model serve as a general model which best describe the drying kinetics of all the three popcorn varieties, with high correlation coefficient. The drying behaviour of the three kernels was found to be largely dependent on changes in temperature and air velocity.

  9. Thin layer modeling of tom yum herbs in vacuum heat pump dryer.

    Science.gov (United States)

    Artnaseaw, A; Theerakulpisut, S; Benjapiyaporn, C

    2010-04-01

    Thin layer vacuum heat pump drying experiments were conducted to determine drying models for Tom Yum herbs (chili, lemon grass, kaffir lime leaf and galangal slice). The drying experiments were conducted in a vacuum heat pump dryer at a constant drying pressure of 0.2 bars and drying temperatures ranging from 50 °C to 65 °C. The experimental results were fitted to a number of well-known thin layer drying models and it was found, for the range of drying temperature tested, that the Midilli model is the best model for all Tom Yum herbs. To account for the influence of drying temperature, the constants and coefficients of model were formulated as functions of the drying temperature. Statistical tests of agreement between the model and experimental results were performed by determining the coefficient of determination (R²) , reduced chi-square (χ²) and root mean square error (RMSE). It was found that the model is in very good agreement with the experimental results.

  10. AN ALTERNATIVE ROUTE TO PRODUCE STANDARDS FOR GEL PERMEATION CHROMATOGRAPHY USING NITROXIDE MEDIATED POLYMERIZATION

    Directory of Open Access Journals (Sweden)

    C. P. R. Malere

    Full Text Available Abstract All over the world standards for Gel Permeation Chromatography (GPC are produced using ionic polymerization. Standards are commercialized in a broad range of molecular weight and their dispersity (Ð must be lower than 1.1. This work proposes the synthesis of polystyrene standards using Nitroxide Mediated Polymerization (NMP, an alternative technique to produce controlled polymers that is much more robust when compared to ionic polymerization. Standards with different ranges of molecular weights were obtained, all of them with very narrow molecular weight distribution (MWD and dispersity (Ð lower than 1.10. In order to do that, several combinations of different initiators were tested. Advanced GPC Triple Detector was used to obtain important properties, such as absolute number and weight average molecular weights, dispersity and intrinsic viscosity. The analytical method used in the characterization of the samples was in-house validated in terms of linearity, accuracy, precision, repeatability and robustness. The validation study demonstrated the quality of the measurements and ensured that the information obtained for a given analyte by the GPC technique is reliable.

  11. Monofluorinated analogues of polybrominated diphenylethers (F-PBDEs) - standards for analysis. Retention behaviour in gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Luthe, G.; Liu, H.; Johansen, J.E. [Chiron Trondheim (Norway); Leonards, P.E.G. [RIVO Ijmuiden (Netherlands)

    2004-09-15

    Polybrominated diphenyl ethers (PBDEs) are globally distributed in the environment. Over the past two decades, they have been used as flame retardants. PBDEs have been found to bioaccumulate. There is a concern about the health effects of PBDE exposure, because of their potential endocrine disrupting properties. PBDEs are structurally similar to polychlorinated biphenyls (PCBs), dibenzodioxines and dibenzofuranes. Therefore, they have to be determined very frequently at the trace level in, e.g. water, food, sediment and soil. The sample preparation and final determination may well lead to systematic and non-systematic (random) errors. It is generally accepted that the accurate determination of micro contaminants in such complex mixtures requires the use of external or, preferably, internal standards (ISs). The benefit of using ISs with physico-chemical properties similar to those of the target compounds, is that both types of errors will be minimized. While preliminary work on monofluorinated polycyclic aromatic hydrocarbons (F-PAHs) as ISs in gas chromatography (GC) was very promising, we recently synthesized a series of monofluorinated polybrominated diphenylethers (F-PBDE). We found that they are a very promising set of internal standards for trace-level analysis of PBDEs and are alternatives to {sup 13}C-labelled analogues. In the present study, we focused attention on the retention behavior of FPBDEs in GC, with the intention to use them as calibration standards for electron impact mass spectrometry (EI-MS) and GC-MS in the negative chemical ionisation mode (ECNI) GC-ECNIMS.

  12. Stability indicating high performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in combined dosage form

    Directory of Open Access Journals (Sweden)

    Deepak Bageshwar

    2011-11-01

    Full Text Available A specific, precise and stability indicating high-performance thin-layer chromatographic method for simultaneous estimation of pantoprazole sodium and itopride hydrochloride in pharmaceutical formulations was developed and validated. The method employed TLC aluminium plates precoated with silica gel 60F254 as the stationary phase. The solvent system consisted of methanol:water:ammonium acetate; 4.0:1.0:0.5 (v/v/v. This system was found to give compact and dense spots for both itopride hydrochloride (Rf value of 0.55±0.02 and pantoprazole sodium (Rf value of 0.85±0.04. Densitometric analysis of both drugs was carried out in the reflectance–absorbance mode at 289 nm. The linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9988±0.0012 in the concentration range of 100–400 ng for pantoprazole sodium. Also, the linear regression analysis data for the calibration plots showed a good linear relationship with R2=0.9990±0.0008 in the concentration range of 200–1200 ng for itopride hydrochloride. The method was validated for specificity, precision, robustness and recovery. Statistical analysis proves that the method is repeatable and selective for the estimation of both the said drugs. As the method could effectively separate the drug from its degradation products, it can be employed as a stability indicating method. Keywords: Gastroesophageal reflux disease (GERD, Itopride hydrochloride, Pantoprazole sodium, High performance thin layer chromatography (HPTLC, Stability indicating, Forced degradation

  13. Fluorine uptake into the human tooth from a thin layer of F-releasing material

    Energy Technology Data Exchange (ETDEWEB)

    Yamamoto, H. [Department of Restorative Dentistry and Endodontology, Graduate School of Dentistry, Osaka University, 1-8 Yamadaoka, Suita, Osaka, 565-0871 (Japan)]. E-mail: yhiroko@dent.osaka-u.ac.jp; Nomachi, M. [Graduate School of Science, Osaka University, Toyonaka, Osaka, 560-0043 (Japan); Yasuda, K. [Wakasa Wan Energy Research Center, Tsuruga, Fukui, 914-0192 (Japan); Iwami, Y. [Department of Restorative Dentistry and Endodontology, Graduate School of Dentistry, Osaka University, 1-8 Yamadaoka, Suita, Osaka, 565-0871 (Japan); Ebisu, S. [Department of Restorative Dentistry and Endodontology, Graduate School of Dentistry, Osaka University, 1-8 Yamadaoka, Suita, Osaka, 565-0871 (Japan); Komatsu, H. [Graduate School of Dental Medicine, Hokkaido University, Sapporo, Hokkaido, 060-8585 (Japan); Sakai, T. [Advanced Radiation Technology Center, JAERI, Takasaki, Gunma, 370-1292 (Japan); Kamiya, T. [Advanced Radiation Technology Center, JAERI, Takasaki, Gunma, 370-1292 (Japan)

    2007-07-15

    Using the proton induced gamma-ray emission (PIGE) method (TIARA, Japan), we have studied fluorine (F) distribution in the human tooth under various conditions. Here, we report F uptake into the human tooth from a thin layer of F-releasing low viscous resin (FLVR). Crowns of human teeth were horizontally cut and the dentin of the cut surface was first covered with four kinds of FLVR (FL-Bond, Reactmer Bond, Xeno Bond, and Protect Liner F; thickness, 50-150 {mu}m) according to the manufacturers' instructions. Non-F-releasing and F-releasing filling resins were also hardened, on the cut surfaces of crowns covered with four kinds of FLVR thin layers. The type of the non-F-releasing filling materials used was LITE FIL IIP: G1-A (FL-Bond and LITE FIL IIP), G2-A (Reactmer Bond and LITE FIL IIP), G3-A (Xeno Bond and LITE FIL IIP), and G4-A (Protect Liner F and LITE FIL IIP). The types of F-releasing filling materials used were G1-B (FL-Bond and Beautifil), G2-B (Reactmer Bond and Reactmer Paste), G3-B (Xeno Bond and Xeno CF Paste), and G4-B (Protect Liner F and Teethmate F-1). Treatment and measurements of specimens were the same as previously reported [H. Yamamoto, M. Nomahci, K. Yasuda, Y. Iwami, S. Ebisu, N. Yamamoto, T. Sakai, T. Kamiya, Nucl. Instr. and Meth. B 210 (2003) 388]. F uptake from specimens following one month of application was estimated from 2-D maps. F penetration was observed in all teeth of G1-A-G4-A groups. The maximum values of F concentration in each tooth and F penetration depth were larger for larger F concentrations in FLVR. FLVR was useful for the F uptake into the tooth, and the F distribution near the thin layer of FLVR depended on the materials used. Between G1-A and G1-B or G4-A and G4-B, the F uptake was significantly different. We were able to obtain fundamental data, which were useful for the analysis of F transportation relating to prevention of caries.

  14. Fluorine uptake into the human tooth from a thin layer of F-releasing material

    Science.gov (United States)

    Yamamoto, H.; Nomachi, M.; Yasuda, K.; Iwami, Y.; Ebisu, S.; Komatsu, H.; Sakai, T.; Kamiya, T.

    2007-07-01

    Using the proton induced gamma-ray emission (PIGE) method (TIARA, Japan), we have studied fluorine (F) distribution in the human tooth under various conditions. Here, we report F uptake into the human tooth from a thin layer of F-releasing low viscous resin (FLVR). Crowns of human teeth were horizontally cut and the dentin of the cut surface was first covered with four kinds of FLVR (FL-Bond, Reactmer Bond, Xeno Bond, and Protect Liner F; thickness, 50-150 μm) according to the manufacturers' instructions. Non-F-releasing and F-releasing filling resins were also hardened, on the cut surfaces of crowns covered with four kinds of FLVR thin layers. The type of the non-F-releasing filling materials used was LITE FIL IIP: G1-A (FL-Bond and LITE FIL IIP), G2-A (Reactmer Bond and LITE FIL IIP), G3-A (Xeno Bond and LITE FIL IIP), and G4-A (Protect Liner F and LITE FIL IIP). The types of F-releasing filling materials used were G1-B (FL-Bond and Beautifil), G2-B (Reactmer Bond and Reactmer Paste), G3-B (Xeno Bond and Xeno CF Paste), and G4-B (Protect Liner F and Teethmate F-1). Treatment and measurements of specimens were the same as previously reported [H. Yamamoto, M. Nomahci, K. Yasuda, Y. Iwami, S. Ebisu, N. Yamamoto, T. Sakai, T. Kamiya, Nucl. Instr. and Meth. B 210 (2003) 388]. F uptake from specimens following one month of application was estimated from 2-D maps. F penetration was observed in all teeth of G1-A-G4-A groups. The maximum values of F concentration in each tooth and F penetration depth were larger for larger F concentrations in FLVR. FLVR was useful for the F uptake into the tooth, and the F distribution near the thin layer of FLVR depended on the materials used. Between G1-A and G1-B or G4-A and G4-B, the F uptake was significantly different. We were able to obtain fundamental data, which were useful for the analysis of F transportation relating to prevention of caries.

  15. The start-to-end chemometric image processing of 2D thin-layer videoscans.

    Science.gov (United States)

    Komsta, Łukasz; Cieśla, Łukasz; Bogucka-Kocka, Anna; Józefczyk, Aleksandra; Kryszeń, Jakub; Waksmundzka-Hajnos, Monika

    2011-05-13

    The purpose of the research was to recommend a unified procedure of image preprocessing of 2D thin layer videoscans for further supervised or unsupervised chemometric analysis. All work was done with open source software. The videoscans saved as JPG files underwent the following procedures: denoising using a median filter, baseline removal with the rollerball algorithm and nonlinear warping using spline functions. The application of the proposed procedure enabled filtration of random difference between images (background intensity changes and spatial differences of the spots location). After the preprocessing only spot intensities have an influence on the performed PCA or other techniques. The proposed technique was successfully applied to recognize the differences between three Carex species from the 2D videoscans of the extracts. The proposed solution may be of value for the any chemometric task--both unsupervised and supervised. Copyright © 2010 Elsevier B.V. All rights reserved.

  16. Mechanism of Thin Layers Graphite Formation by 13C Implantation and Annealing

    Directory of Open Access Journals (Sweden)

    Gaelle Gutierrez

    2014-04-01

    Full Text Available The mechanism of thin layers graphite (TLG synthesis on a polycrystalline nickel film deposited on SiO2 (300 nm thick/Si(100 has been investigated by 13C implantation of four equivalent graphene monolayers and annealing at moderate temperatures (450–600 °C. During this process, the implanted 13C segregates to the surface. Nuclear Reaction Analyses (NRA are used for the first time in the topic of graphene synthesis to separate the isotopes and to determine the 12C and 13C concentrations at each step. Indeed, a significant part of carbon in the TLG also comes from residual 12C carbon absorbed into the metallic matrix. Raman spectroscopy and imaging are used to determine the main location of each carbon isotope in the TLG. The Raman mappings especially emphasize the role of 12C previously present at the surface that first diffuses along grain boundaries. They play the role of nucleation precursors. Around them the implanted 13C or a mixture of bulk 12C–13C aggregate and further precipitate into graphene-like fragments. Graphenization is effective at around 600 °C. These results point out the importance of controlling carbon incorporation, as well as the importance of preparing a uniform nickel surface, in order to avoid heterogeneous nucleation.

  17. Removal of long-lived {sup 222}Rn daughters by electropolishing thin layers of stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Schnee, R. W.; Bowles, M. A.; Bunker, R.; McCabe, K.; White, J. [Department of Physics, Syracuse University, Syracuse, NY 13244 (United States); Cushman, P.; Pepin, M. [School of Physics and Astronomy, University of Minnesota, Minneapolis, MN 55455 (United States); Guiseppe, V. E. [University of South Dakota, Vermillion, South Dakota 57069 (United States)

    2013-08-08

    Long-lived alpha and beta emitters in the {sup 222}Rn decay chain on detector surfaces may be the limiting background in many experiments attempting to detect dark matter or neutrinoless double beta decay. Removal of tens of microns of material via electropolishing has been shown to be effective at removing radon daughters implanted into material surfaces. Some applications, however, require the removal of uniform and significantly smaller thicknesses. Here, we demonstrate that electropolishing < 1 μm from stainless-steel plates reduces the contamination efficiently, by a factor > 100. Examination of electropolished wires with a scanning electron microscope confirms that the thickness removed is reproducible and reasonably uniform. Together, these tests demonstrate the effectiveness of removal of radon daughters for a proposed low-radiation, multi-wire proportional chamber (the BetaCage), without compromising the screener’s energy resolution. More generally, electropolishing thin layers of stainless steel may effectively remove radon daughters without compromising precision-machined parts.

  18. Computer-aided identifications of thin-layer chromatographic patterns in broad-spectrum drug screening.

    Science.gov (United States)

    Siek, T J; Stradling, C W; McCain, M W; Mehary, T C

    1997-04-01

    We have developed a systematic thin-layer chromatographic (TLC) technique for detecting and identifying drugs and drug metabolites on 10-cm-long silica-gel plates with organic binder (fluorescent indicator); a computer program (SPOT CHEK) assists in matching the data from a particular chromatogram with those obtained for known drugs recovered from serum, urine, or other specimens. The plates are developed in a single mobile phase. Visualization and detection reagents used to characterize unknowns include fluorescamine, ferric chloride/perchloric acid/nitric acid, Dragendorff, Marquis, Mandelin, and iodinated Dragendorff solutions, 254 nm ultraviolet light, and vapor from chlorine or hydrochloric acid. Detection limits of 5-200 ng per sample spot were obtained for drugs in the database. The computer program database is based on nine reaction responses plus the plate zone locations for 243 drug substances but requires entry of only one TLC property to generate a matching list. We ran the program with an IBM-compatible 386/486 PC using an MS-DOS operating system (version 6.2).

  19. Thin layer convective solar drying and mathematical modeling of prickly pear peel (Opuntia ficus indica)

    Energy Technology Data Exchange (ETDEWEB)

    Lahsasni, S.; Mahrouz, M. [Unite de Chimie Agroalimentaire (LCOA), Faculte des Sciences Semlalia, Marrakech (Morocco); Kouhila, M.; Idlimam, A.; Jamali, A. [Ecole Normale Superieure, Marrakech (Morocco). Lab. d' Energie Solaire et Plantes Aromatiques et Medicinales

    2004-02-01

    This paper presents the thin layer convective solar drying and mathematical modeling of prickly pear peel. For these purposes, an indirect forced convection solar dryer consisting of a solar air collector, an auxiliary heater, a circulation fan and a drying cabinet is used for drying experiments. Moreover, the prickly pear peel is sufficiently dried in the ranges of 32 to 36 {sup o} C of ambient air temperature, 50 to 60 {sup o}C of drying air temperature, 23 to 34% of relative humidity, 0.0277 to 0.0833 m{sup 3}/s of drying air flow rate and 200 to 950 W/m{sup 2} of daily solar radiation. The experimental drying curves show only a falling drying rate period. The main factor in controlling the drying rate was found to be the drying air temperature. The drying rate equation is determined empirically from the characteristic drying curve. Also, the experimental drying curves obtained were fitted to a number of mathematical models. The Midilli-Kucuk drying model was found to satisfactorily describe the solar drying curves of prickly pear peel with a correlation coefficient (r) of 0.9998 and chi-square ({chi}{sup 2}) of 4.6572 10{sup -5}. (Author)

  20. Electrode polarization and unusual magnetodielectric effect in a transformer oil-based magnetic nanofluid thin layer.

    Science.gov (United States)

    Rajnak, Michal; Dolnik, Bystrik; Kurimsky, Juraj; Cimbala, Roman; Kopcansky, Peter; Timko, Milan

    2017-01-07

    In the present paper, we provide low-frequency dielectric spectra for a thin layer of a nanofluid based on transformer oil and iron oxide nanoparticles stabilized by oleic acid. The complex dielectric permittivity measured in the frequency range from 1 mHz to 200 kHz shows an obvious electrode polarization effect and a Debye-like dielectric relaxation process. Both effects stem from the presence of space charge in the oil due to impurity ions, and in the nanofluid represented predominantly by a residual surfactant and uncompensated particle surface charge. It is shown that the spectra, which were measured in the temperature range from 298 K to 358 K, can be well represented by a fitting function consisted of one Havriliak-Negami term and the Jonscher's power law. In the investigated magnetic nanofluid layer, we found that the onset of the electrode polarization is suppressed to lower frequencies by the application of an external magnetic field (300 mT). This phenomenon is explained by a slowed-down migration of the space charge due to the Lorentz force and by a hindering effect of the formed magnetic nanoparticle aggregates. Surprisingly, a moderate decrease in the whole permittivity spectrum was observed for both parallel and perpendicular orientations of the electric and magnetic fields. This is in contradiction with the usual magnetodielectric anisotropy effect. Based on our qualitative analysis, we discuss potential reasons accountable for the observed effect.

  1. Thin layer drying of wormwood ( Artemisia absinthium L.) leaves: dehydration characteristics, rehydration capacity and energy consumption

    Science.gov (United States)

    Beigi, Mohsen

    2017-08-01

    This study aimed at determining the influence of temperature on drying, rehydration and consumed energy characteristics of common wormwood leaves during thin layer drying. The experiments were carried out at temperatures of 50, 60 and 70 °C and a constant air velocity of 0.7 m s-1. The dehydration duration decreased significantly with increasing drying air temperature. The usefulness of five different mathematical models to simulate the experimental drying kinetics was evaluated and the Midilli model was found to be the best model for explaining the curves. Effective moisture diffusivity values were obtained to be in the range of 7.099 × 10-8-3.191 × 10-7 m2 s-1. Rehydration capacity of the dried leaves increased with increasing rehydration water temperature and decreasing drying air temperature. The specific energy consumption decreased with any increment in drying air temperature and varied from 17.64 to 32.09 kWh kg-1.

  2. Atomically thin layered NiFe double hydroxides assembled 3D microspheres with promoted electrochemical performances

    Science.gov (United States)

    Li, Xiaomin; Zai, Jiantao; Liu, Yuanyuan; He, Xiaobo; Xiang, Shijie; Ma, Zifeng; Qian, Xuefeng

    2016-09-01

    LDHs in atomic thickness (mono-/bi-layers) usually exhibit novel physicochemical properties, especially in surface-dependent energy storage and catalysis areas. However, the thickness of the commonly reported 2D LDHs is in nanoscale and the bottom-up synthesis of atomically thin LDHs is rarely reported. Herein, high-quality atomically thin layered NiFe-LDHs assembled 3D microspheres were synthesized via a rational designed reaction system, where the formation of atomically thin building blocks was controlled by the synergetic effects of released carbonate anions and butanol. Furthermore, the complexant and solvents played important effects on the process of coprecipitation and the assembling of LDHs. Due to the nature of atomically thin LDHs nanosheets and unique 3D hierarchical structures, the obtained microspheres exhibited excellent electrocatalytic oxygen evolution reaction (OER) activity in alkaline medium with an onset overpotential (0.435 V, which is lower than that of common LDHs) and good durability. The as-prepared 3D NiFe-LDHs microspheres were also firstly used as supercapacitor materials and displayed a high specific capacitance of 1061 F g-1 at the current density of 1 A g-1.

  3. Thin-layer chromatographic identification of Chinese propolis using chemometric fingerprinting.

    Science.gov (United States)

    Tang, Tie-xin; Guo, Wei-yan; Xu, Ye; Zhang, Si-ming; Xu, Xin-jun; Wang, Dong-mei; Zhao, Zhi-min; Zhu, Long-ping; Yang, De-po

    2014-01-01

    Poplar tree gum has a similar chemical composition and appearance to Chinese propolis (bee glue) and has been widely used as a counterfeit propolis because Chinese propolis is typically the poplar-type propolis, the chemical composition of which is determined mainly by the resin of poplar trees. The discrimination of Chinese propolis from poplar tree gum is a challenging task. To develop a rapid thin-layer chromatographic (TLC) identification method using chemometric fingerprinting to discriminate Chinese propolis from poplar tree gum. A new TLC method using a combination of ammonia and hydrogen peroxide vapours as the visualisation reagent was developed to characterise the chemical profile of Chinese propolis. Three separate people performed TLC on eight Chinese propolis samples and three poplar tree gum samples of varying origins. Five chemometric methods, including similarity analysis, hierarchical clustering, k-means clustering, neural network and support vector machine, were compared for use in classifying the samples based on their densitograms obtained from the TLC chromatograms via image analysis. Hierarchical clustering, neural network and support vector machine analyses achieved a correct classification rate of 100% in classifying the samples. A strategy for TLC identification of Chinese propolis using chemometric fingerprinting was proposed and it provided accurate sample classification. The study has shown that the TLC identification method using chemometric fingerprinting is a rapid, low-cost method for the discrimination of Chinese propolis from poplar tree gum and may be used for the quality control of Chinese propolis. Copyright © 2014 John Wiley & Sons, Ltd.

  4. Development of counting system for wear measurements using Thin Layer Activation and the Wearing Apparatus

    Energy Technology Data Exchange (ETDEWEB)

    França, Michel de A.; Suita, Julio C.; Salgado, César M., E-mail: mchldante@gmail.com, E-mail: suita@ien.gov.br, E-mail: otero@ien.gov.br [Instituto de Engenharia Nuclear (IEN/CNEN-RJ), Rio de Janeiro, RJ (Brazil)

    2017-07-01

    This paper focus on developing a counting system for the Wearing Apparatus, which is a device previously built to generate measurable wear on a given surface (Main Source) and to carry the fillings from it to a filter (second source). The Thin Layer Activation is a technique used to produce activity on one of the Wearing Apparatus' piece, this activity is proportional to the amount of material worn, or scrapped, from the piece's surface. Thus, by measuring the activity on those two points it is possible to measure the produced wear. The methodology used in this work is based on simulations through MCNP-X Code to nd the best specifications for shielding, solid angles, detectors dimensions and collimation for the Counting System. By simulating several scenarios, each one different from the other, and analyzing the results in the form of Counts Per Second, the ideal counting system's specifications and geometry to measure the activity in the Main Source and the Filter (second source) is chosen. After that, a set of previously activated stainless steel foils were used to reproduce the real experiments' conditions, this real experiment consists of using TLA and the Wearing Apparatus, the results demonstrate that the counting system and methodology are adequate for such experiments. (author)

  5. Thin layer thickness measurements by zero group velocity Lamb mode resonances

    Science.gov (United States)

    Cès, Maximin; Clorennec, Dominique; Royer, Daniel; Prada, Claire

    2011-11-01

    Local and non-contact measurements of the thickness of thin layers deposited on a thick plate have been performed by using zero group velocity (ZGV) Lamb modes. It was shown that the shift of the resonance frequency is proportional to the mass loading through a factor which depends on the mechanical properties of the layer and of the substrate. In the experiments, ZGV Lamb modes were generated by a Nd:YAG pulsed laser and the displacement normal to the plate surface was measured by an optical interferometer. Measurements performed at the same point that the generation on the non-coated face of the plate demonstrated that thin gold layers of a few hundred nanometers were detected through a 1.5-mm thick Duralumin plate. The shift of the resonance frequency (1.9 MHz) of the fundamental ZGV mode is proportional to the layer thickness: typically 10 kHz per μm. Taking into account the influence of the temperature, a 240-nm gold layer was measured with a ±4% uncertainty. This thickness has been verified on the coated face with an optical profiling system.

  6. Thin layer drying kinetics of by-products from olive oil processing.

    Science.gov (United States)

    Montero, Irene; Miranda, Teresa; Arranz, Jose Ignacio; Rojas, Carmen Victoria

    2011-01-01

    The thin-layer behavior of by-products from olive oil production was determined in a solar dryer in passive and active operation modes for a temperature range of 20-50 °C. The increase in the air temperature reduced the drying time of olive pomace, sludge and olive mill wastewater. Moisture ratio was analyzed to obtain effective diffusivity values, varying in the oil mill by-products from 9.136 × 10(-11) to 1.406 × 10(-9) m(2)/s in forced convection (m(a) = 0.22 kg/s), and from 9.296 × 10(-11) to 6.277 × 10(-10) m(2)/s in natural convection (m(a) = 0.042 kg/s). Diffusivity values at each temperature were obtained using the Fick's diffusion model and, regardless of the convection, they increased with the air temperature. The temperature dependence on the effective diffusivity was determined by an Arrhenius type relationship. The activation energies were found to be 38.64 kJ/mol, 30.44 kJ/mol and 47.64 kJ/mol for the olive pomace, the sludge and the olive mill wastewater in active mode, respectively, and 91.35 kJ/mol, 14.04 kJ/mol and 77.15 kJ/mol in natural mode, in that order.

  7. Investigation of anti-wear performance of automobile lubricants using thin layer activation analysis technique

    Energy Technology Data Exchange (ETDEWEB)

    Biswal, Jayashree [Isotope and Radiation Application Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Thakre, G.D. [Tribology and Combustion Division, Indian Institute of Petroleum, Dehradun 248005, Uttarakhand (India); Pant, H.J., E-mail: hjpant@barc.gov.in [Isotope and Radiation Application Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Samantray, J.S. [Isotope and Radiation Application Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Arya, P.K. [Tribology and Combustion Division, Indian Institute of Petroleum, Dehradun 248005, Uttarakhand (India); Sharma, S.C.; Gupta, A.K. [Nuclear Physics Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India)

    2017-05-15

    An investigation was carried out to examine the anti-wear behavior of automobile lubricants using thin layer activation analysis technique. For this study disc gears made of EN 31 steel were labeled with a small amount of radioactivity by irradiating with 13 MeV proton beam from a particle accelerator. Experiments on wear rate measurement of the gear were carried out by mounting the irradiated disc gear on a twin-disc tribometer under lubricated condition. The activity loss was monitored by using a NaI(Tl) scintillation detector integrated with a multichannel analyzer. The relative remnant activity was correlated with thickness loss by generating a calibration curve. The wear measurements were carried out for four different types of lubricants, named as, L1, L2, L3 and L4. At lower load L1 and L4 were found to exhibit better anti-wear properties than L2 and L3, whereas, L4 exhibited the best anti-wear performance behavior than other three lubricants at all the loads and speeds investigated.

  8. Separation of Berberine Hydrochloride and Tetrahydropalmatine and Their Quantitative Analysis with Thin Layer Chromatography Involved with Ionic Liquids

    National Research Council Canada - National Science Library

    Lu, Jing; Ma, Hong-yan; Zhang, Wei; Ma, Zhi-guo; Yao, Shun

    2015-01-01

    .... Supported imidazole ionic liquid with hydroxide ion on silica gel (SiO2·Im+·OH−) was synthesized through simple procedure and characterized by Fourier transform infrared spectroscopy (FT-IR...

  9. INVESTIGATION OF A MIXTURE CONTAINING ALPRAZOLAM, CODEINE AND PARACETAMOL USING THIN-LAYER AND HIGH PERFORMANCE LIQUID CHROMATOGRAPHY METHODS.

    Science.gov (United States)

    Ciegis, Paulius; Zevzikovas, Andrejus; Zevzikoviene, Augusta; Nenortiene, Palma; Kazlauskiene, Daiva

    2016-01-01

    The increasing drug consumption in Lithuania and all over the world makes us think about the negative consequences - the risk of toxicity. Fast and accurate identification of material that caused the poisoning reduces the probability in death cases and makes easier to determine the main cause of death. The results have shown that the most appropriate systems of solvents for qualitative analysis by TLC method of the mixture consisting of alprazolam, codeine and paracetanol are: system "D" (trichloromethane : acetone : conc. ammonia = 55 : 40 : 5 (v/v/v)) and system "F" (trichloromethane : diethyl ether: isobutanol : conc. ammonia = 50 : 30 : 15 : 5 (v/v/v/v)). For qualitative analysis of the mixture consisting of alprazolam, codeine and paracetamol by HPLC method the chromatographic column ACE C18 (25 cm x 4.6 mm x 5 µm), gradient elution mode (mixture of 3% acetic acid and methanol and the flow rate 1 mL/min have been used. The injection volume was 10 pL. Photodiode array detector (210 - 240 nm range) has been used. UV absorption spectra of materials measured using photodiode array detector have been identical to those presented in the scientific literature.

  10. A technique for extraction and Thin Layer Chromatography visualization of fecal bile acids applied to neotropical felid scats

    Directory of Open Access Journals (Sweden)

    Ada Virginia Cazón Narvaez

    1999-06-01

    Full Text Available Fecal bile acid patterns have been used successfully to identify scats. Neotropical felid scats are capable of this biochemical identification because they present low concentrations of plant pigments that would interfere in fecal bile acids detection. However, neotropical felid scats have poor quantities of bile acids, so we developed in this work a proper technique for their extraction, visualization and determination. Twenty eighth feces of seven different felid species, collected from Zoological and Wildlife Parks, were dried and pulverized. The procedure for analyzing feces is : Take one g of pulverized feces and shake for 3 hr at room temperature in 20 ml benzene : methanol; filter and evaporate to 5 ml. Spot on TLC plate and develop in toluene :acetic acid:water. Dry and visualize with anisaldehyde. Field collected scats could be identified by the bile acids pattern revealed by this specific technique and ,then, used as a source of information for distribution, density and food habits studies.Los patrones de ácidos biliares fecales han sido utilizados satisfactoriamente para identificar heces. Las heces de félidos neotropicales son propicias para ser identificadas bioquímicamente, ya que contienen baja concentración de pigmentos vegetales que pudieran interferir en la detección de ácidos biliares. Sin embargo los ácidos biliares se encuentran en bajas concentraciones en las heces, por lo cual desarrollamos en este trabajo una técnica apropiada para su extracción, visualización y determinación. Veintiocho heces de diferentes félidos recolectadas de Zoológicos y Estaciones de Fauna Silvestre fueron secadas y pulverizadas. El procedimiento para analizar las heces es : Tomar un gramo de feca pulverizada y agitar en 20 ml de benceno :metanol a temperatura ambiente durante 3 hr ; luego filtrar y evaporar hasta 5 ml. Sembrar en placa de TLC y desarrollar en tolueno :ác. acético :agua. Secar y revelar con anisaldehído. Las heces recolectadas en el campo podrían ser identificadas a través de los patrones de ácidos biliares evidenciados con esta técnica específica, y ser entonces utilizadas como fuente de información en estudios sobre distribución, densidad y hábito alimenticio.

  11. Validation of a Thin-Layer Chromatography for the Determination of Hydrocortisone Acetate and Lidocaine in a Pharmaceutical Preparation

    Directory of Open Access Journals (Sweden)

    Małgorzata Dołowy

    2014-01-01

    Full Text Available A new specific, precise, accurate, and robust TLC-densitometry has been developed for the simultaneous determination of hydrocortisone acetate and lidocaine hydrochloride in combined pharmaceutical formulation. The chromatographic analysis was carried out using a mobile phase consisting of chloroform + acetone + ammonia (25% in volume composition 8 : 2 : 0.1 and silica gel 60F254 plates. Densitometric detection was performed in UV at wavelengths 200 nm and 250 nm, respectively, for lidocaine hydrochloride and hydrocortisone acetate. The validation of the proposed method was performed in terms of specificity, linearity, limit of detection (LOD, limit of quantification (LOQ, precision, accuracy, and robustness. The applied TLC procedure is linear in hydrocortisone acetate concentration range of 3.75÷12.50 μg·spot−1, and from 1.00÷2.50 μg·spot−1 for lidocaine hydrochloride. The developed method was found to be accurate (the value of the coefficient of variation CV [%] is less than 3%, precise (CV [%] is less than 2%, specific, and robust. LOQ of hydrocortisone acetate is 0.198 μg·spot−1 and LOD is 0.066 μg·spot−1. LOQ and LOD values for lidocaine hydrochloride are 0.270 and 0.090 μg·spot−1, respectively. The assay value of both bioactive substances is consistent with the limits recommended by Pharmacopoeia.

  12. Validation of a Thin-Layer Chromatography for the Determination of Hydrocortisone Acetate and Lidocaine in a Pharmaceutical Preparation

    Science.gov (United States)

    Dołowy, Małgorzata; Kulpińska-Kucia, Katarzyna; Pyka, Alina

    2014-01-01

    A new specific, precise, accurate, and robust TLC-densitometry has been developed for the simultaneous determination of hydrocortisone acetate and lidocaine hydrochloride in combined pharmaceutical formulation. The chromatographic analysis was carried out using a mobile phase consisting of chloroform + acetone + ammonia (25%) in volume composition 8 : 2 : 0.1 and silica gel 60F254 plates. Densitometric detection was performed in UV at wavelengths 200 nm and 250 nm, respectively, for lidocaine hydrochloride and hydrocortisone acetate. The validation of the proposed method was performed in terms of specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, and robustness. The applied TLC procedure is linear in hydrocortisone acetate concentration range of 3.75 ÷ 12.50 μg·spot−1, and from 1.00 ÷ 2.50 μg·spot−1 for lidocaine hydrochloride. The developed method was found to be accurate (the value of the coefficient of variation CV [%] is less than 3%), precise (CV [%] is less than 2%), specific, and robust. LOQ of hydrocortisone acetate is 0.198 μg·spot−1 and LOD is 0.066 μg·spot−1. LOQ and LOD values for lidocaine hydrochloride are 0.270 and 0.090 μg·spot−1, respectively. The assay value of both bioactive substances is consistent with the limits recommended by Pharmacopoeia. PMID:24526880

  13. Frontal elution and frontal displacement methods in thin-layer chromatography and their use in concentrating of impurities

    Science.gov (United States)

    Berezkin, V. G.; Chausov, A. V.

    2011-10-01

    A new method of TLC is proposed for concentrating and separating diluted solutions of samples. Samples being analyzed are concentrated in a narrow band on a plate using the displacement version of TLC the aim of lowering the detection limit of the impurities. We compare the frontal elution described in the first work on TLC by Izmailov and Shraiber with the frontal displacement suggested in this work for concentrating diluted solutions of samples and their further separation by linear TLC. It is demonstrated that using displacement TLC in the analytical process allows us to raise the efficiency of separating the compounds under study, and to lower their detection limit by a factor of 103. We conclude that the use of this approach for the determination of impurities in TLC is advisable in analytical practice.

  14. The Development of a Tool for Measuring Graduate Students' Topic Specific Pedagogical Content Knowledge of Thin Layer Chromatography

    Science.gov (United States)

    Hale, L. V. A.; Lutter, J. C.; Shultz, G. V.

    2016-01-01

    Graduate students play a critical role in undergraduate education at doctorate granting institutions; but generally have minimal opportunity to develop teaching expertise. Furthermore, little is known about how graduate students develop teaching expertise in this context. We investigated the development of topic-specific pedagogical content…

  15. Fluorescence detection by intensity changes for high-performance thin-layer chromatography separation of lipids using automated multiple development.

    Science.gov (United States)

    Cebolla, Vicente L; Jarne, Carmen; Domingo, Pilar; Domínguez, Andrés; Delgado-Camón, Aránzazu; Garriga, Rosa; Galbán, Javier; Membrado, Luis; Gálvez, Eva M; Cossío, Fernando P

    2011-05-13

    Changes in emission of berberine cation, induced by non-covalent interactions with lipids on silica gel plates, can be used for detecting and quantifying lipids using fluorescence scanning densitometry in HPTLC analysis. This procedure, referred to as fluorescence detection by intensity changes (FDIC) has been used here in combination with automated multiple development (HPTLC/AMD), a gradient-based separation HPTLC technique, for separating, detecting and quantifying lipids from different families. Three different HPTLC/AMD gradient schemes have been developed for separating: neutral lipid families and steryl glycosides; different sphingolipids; and sphingosine-sphinganine mixtures. Fluorescent molar responses of studied lipids, and differences in response among different lipid families have been rationalized in the light of a previously proposed model of FDIC response, which is based on ion-induced dipole interactions between the fluorophore and the analyte. Likewise, computational calculations using molecular mechanics have also been a complementary useful tool to explain high FDIC responses of cholesteryl and steryl-derivatives, and moderate responses of sphingolipids. An explanation for the high FDIC response of cholesterol, whose limit of detection (LOD) is 5 ng, has been proposed. Advantages and limitations of FDIC application have also been discussed. Copyright © 2010 Elsevier B.V. All rights reserved.

  16. Peptide dot immunoassay and immunoblotting: electroblotting from aluminum thin-layer chromatography plates and isoelectric focusing gels to activated nitrocellulose

    DEFF Research Database (Denmark)

    Bjerrum, O.J.; Holm, A.; Lauritzen, Edgar

    1993-01-01

    Peptide dot immunoassay, electroblotting, activated nitrocellulose, dot blot, membranes, peptides and proteins......Peptide dot immunoassay, electroblotting, activated nitrocellulose, dot blot, membranes, peptides and proteins...

  17. Analytical Method Validation and Determination of Pyridoxine, Nicotinamide, and Caffeine in Energy Drinks Using Thin Layer Chromatography-Densitometry

    Directory of Open Access Journals (Sweden)

    Florentinus Dika Octa Riswanto

    2015-03-01

    Full Text Available Food supplement which contains vitamins and stimulants such as caffeine were classified as energy drink. TLC-densitometry method was chosen to determine the pyridoxine, nicotinamide, and caffeine in the energy drink sample. TLC plates of silica gel 60 F254 was used as the stationary phase and methanol : ethyl acetate : ammonia 25% (134:77:10 was used as the mobile phase. The correlation coefficient for each pyridoxine, nicotinamide, and caffeine were 0.9982, 0.9997, and 0.9966, respectively. Detection and quantitation limits of from the three analytes were 4.05 and 13.51 µg/mL; 13.15 and 43.83 µg/mL; 5.43 and 18.11 µg/mL, respectively. The recovery of pyridoxine, nicotinamide, and caffeine were within the required limit range of 95-105%. The percent of RSD were below the limit value of 5.7% for caffeine and nicotinamide and 8% for pyridoxine. The content amount of pyridoxine in the sample 1 and 2 were 33.59 ± 0.981 and 30.29 ± 2.061 µg/mL, respectively. The content amount of nicotinamide in the sample 1 and 2 were 106.53 ± 3.521 and 98.20 ± 3.648 µg/mL, respectively. The content amount of caffeine in the sample 1 and 2 were 249.50 ± 5.080 and 252.80 ± 2.640 µg/mL, respectively. Robustness test results showed that the most optimal method conditions should be applied for the analysis.

  18. Thin-Layer Chromatography of 2-Imino-3-(Substituted Aryl)-1-Thiazolidin- 4-Ones and Their Intermediates, Chloroacetanilides

    OpenAIRE

    Minbale Aschale

    2014-01-01

    International Journal of Engineering Research and Applications (IJERA) is an open access online peer reviewed international journal that publishes research and review articles in the fields of Computer Science, Neural Networks, Electrical Engineering, Software Engineering, Information Technology, Mechanical Engineering, Chemical Engineering, Plastic Engineering, Food Technology, Textile Engineering, Nano Technology & science, Power Electronics, Electronics & Communication Engineering, Computa...

  19. Comparison of the separation of nine tryptamine standards based on gas chromatography, high performance liquid chromatography and capillary electrophoresis methods.

    Science.gov (United States)

    Wang, Man-Juing; Liu, Ju-Tsung; Chen, Hung-Ming; Lin, Jian-Jhih; Lin, Cheng-Huang

    2008-02-15

    Nine tryptamines, including alpha-methyltryptamine (AMT), N,N-dimethyltryptamine (DMT), 5-methoxy-alpha-methyltryptamine (5-MeO-AMT), N,N-diethyltryptamine (DET), N,N-dipropyltryptamine (DPT), N,N-dibutyltryptamine (DBT), N,N-diisopropyltryptamine (DIPT), 5-methoxy-N,N-dimethyltryptamine (5-MeO-DMT), and 5-methoxy-N,N-diisopropyltryptamine (5-MeO-DIPT) were selected as model compounds. Comparisons of their sensitivity, selectivity, time, cost and the order of migration are described based on different separation techniques (GC, HPLC and CE, respectively). As a result, the limit of detection (S/N=3) obtained by GC/MS and LC/UV-absorption ranged from 0.5 to 15 microg/mL and 0.3 to 1.0 microg/mL, respectively. In contrast to this, based on the CZE/UV-absorption method, the limit of detection (S/N=3) was determined to 0.5-1 microg/mL. However, when the sweeping-MEKC mode was applied, it dramatically improved to 2-10 ng/mL. In the case of GC, HPLC and CE, migration times of the nine standards ranged from 11 to 15 min and 8 to 23 min by GC and HPLC, respectively; ranged from 20 to 26 min by sweeping-MEKC. The order of migration of DMT, DET, DPT and DBT follows the molecular weight, whereas the order of migration of AMT and 5-MeO-AMT (primary amines), DIPT (an isomer of DPT) and 5-methoxy-tryptamines (5-MeO-AMT, 5-MeO-DMT and 5-MeO-DIPT) can be altered by changing the separation conditions.

  20. Mathematical modelling of thin layer drying process of long green pepper in solar dryer and under open sun

    Energy Technology Data Exchange (ETDEWEB)

    Akpinar, E. Kavak; Bicer, Y. [Mechanical Engineering Department, Firat University, 23279 Elazig (Turkey)

    2008-06-15

    An experimental study was performed to determine the thin layer drying characteristics in a solar dryer with forced convection and under open sun with natural convection of long green pepper. An indirect forced convection solar dryer consisting of a solar air collector and drying cabinet was used in the experiments. Natural sun drying experiments were conducted for comparison at the same time. The constant rate period is absent from the drying curves. The drying process took place in the falling rate period. The drying data were fitted to 13 different mathematical models. Among the models, the logarithmic model for forced solar drying and the Midilli and Kucuk model for natural sun drying were found best to explain the thin layer drying behaviour of long green peppers. The performance of these models was investigated by comparing the coefficient of determination (R), reduced chi-square ({chi}{sup 2}) and root mean square error (RMSE) between the observed and predicted moisture ratios. (author)

  1. Measuring the Corrosion Rate of Aluminum by Using Ultra Thin Layer Activation Technique

    Directory of Open Access Journals (Sweden)

    I. Kambali

    2005-01-01

    Full Text Available Corrosion rate of aluminum (99.9% purity in 0.001 M hydrochloride acid solution has been measured by using Ultra Thin Layer Activation (UTLA technique. Iron foil of 25 μm thickness was used as the primary target and activated by 10.2 MeV proton beam coming from BATAN’s cyclotron with irradiation dose of 0.73 μAh (9.534 x 1015 protons/cm2. Radioisotope 56Co formed on the foil would have sufficient kinetic energy to run out of the foil’s surface and be implanted on the aluminum used as the secondary target. After 2 days of cooling down, about 0.397 MBq of 56Co stayed on the foil was counted by NaI(Tl detector coupled with Multi Channel Analyzer (MCA.It was found that about 9.45% of the total 56Co formed on the iron foil was successfully implanted into aluminum target. Corrosion test of aluminum was conducted in a 2 inches diameter pipe filled with 0.001 M hydrochloride acid flowing with a rate of 80 liters/minute. The corrosion rate of the aluminum was determined from the change of 56Co activity during the process. The result of experiment indicated that the sample was corroded with a very slow rate of 0.064 nm/minute and 0.0054 nm/minute for measuring time of 0-180 and 180-300 minutes respectively.

  2. Thin-layer infrared spectroscopic study on thermal behavior of non-phospholipid lipids and nanovesicles

    Science.gov (United States)

    Bista, Rajan K.; Bruch, Reinhard F.; Covington, Aaron M.

    2009-02-01

    °The investigation of thermal behaviors and subsequent changes in the conformational order of lipids and liposomes is of importance in understanding various phenomena such as the formation and fusion of vesicles, trans-membrane diffusion and membrane interactions with drugs and proteins. In this work, the thermal behavior of a suite of newly developed self-forming synthetic non-phospholipid (PEGylated) lipids and its nanovesicles in buffer suspensions were investigated by variable-temperature thin-layered Fourier Transform Infrared (FTIR) transmission spectroscopy. The temperature-induced infrared spectra of such lipids composed of 1,2-dimyristoyl-rac-glycerol-3-dodecaethylene glycol (GDM-12) and 1,2-distearoyl-rac-glycerol-3-triicosaethylene glycol (GDS-23) were acquired by using FTIR spectrometer in conjunction with a custom built temperature-controlled demountable liquid cell. In contrast to conventional phospholipids, these novel lipids form liposomes spontaneously upon hydration, without the supply of external activation energy. It was found that the thermal stability of the PEGylated lipids defer greatly depending upon the acyl chain-lengths as well as number of associated head group units. Particularly, GDM-12 (saturated 14 hydrocarbon chains) shows one sharp order-disorder transition with temperature increasing from 3 to 5 °C. Similarly, GDS-23 (saturated 18 hydrocarbon chains) exhibits comparatively broad order-disorder transition profiles between temperature 17 and 22 °C. However, the phase transition temperature becomes significantly higher for lipid nanovesicles formed in aqueous suspensions. The results obtained in this study may find applications in various areas including the development of lipid based substance and drug delivery systems.

  3. Microporous Polyurethane Thin Layer as a Promising Scaffold for Tissue Engineering

    Directory of Open Access Journals (Sweden)

    Justyna Kucińska-Lipka

    2017-07-01

    Full Text Available The literature describes that the most efficient cell penetration takes place at 200–500 µm depth of the scaffold. Many different scaffold fabrication techniques were described to reach these guidelines. One such technique is solvent casting particulate leaching (SC/PL. The main advantage of this technique is its simplicity and cost efficiency, while its main disadvantage is the scaffold thickness, which is usually not less than 3000 µm. Thus, the scaffold thickness is usually far from the requirements for functional tissue reconstruction. In this paper, we report a successful fabrication of the microporous polyurethane thin layer (MPTL of 1 mm thick, which was produced using SC/PL technique combined with phase separation (PS. The obtained MPTL was highly porous (82%, had pore size in the range of 65–426 µm and scaffold average pore size was equal to 154 ± 3 µm. Thus, it can be considered a suitable scaffold for tissue engineering purpose, according to the morphology criterion. Polyurethane (PUR processing into MPTL scaffold caused significant decrease of contact angle from 78 ± 4° to 56 ± 6° and obtained MPTL had suitable hydrophilic characteristic for mammalian cells growth and tissue regeneration. Mechanical properties of MPTL were comparable to the properties of native tissues. As evidenced by biotechnological examination the MPTL were highly biocompatible with no observed apparent toxicity on mouse embryonic NIH 3T3 fibroblast cells. Performed studies indicated that obtained MPTL may be suitable scaffold candidate for soft TE purposes such as blood vessels.

  4. Cleaning of conveyor belt materials using ultrasound in a thin layer of water.

    Science.gov (United States)

    Axelsson, L; Holck, A; Rud, I; Samah, D; Tierce, P; Favre, M; Kure, C F

    2013-08-01

    Cleaning of conveyor belts in the food industry is imperative for preventing the buildup of microorganisms that can contaminate food. New technologies for decreasing water and energy consumption of cleaning systems are desired. Ultrasound can be used for cleaning a wide range of materials. Most commonly, baths containing fairly large amounts of water are used. One possibility to reduce water consumption is to use ultrasonic cavitation in a thin water film on a flat surface, like a conveyor belt. In order to test this possibility, a model system was set up, consisting of an ultrasound transducer/probe with a 70-mm-diameter flat bottom, operating at 19.8 kHz, and contaminated conveyor belt materials in the form of coupons covered with a thin layer of water or water with detergent. Ultrasound was then applied on the water surface at different power levels (from 46 to 260 W), exposure times (10 and 20 s), and distances (2 to 20 mm). The model was used to test two different belt materials with various contamination types, such as biofilms formed by bacteria in carbohydrate- or protein-fat-based soils, dried microorganisms (bacteria, yeasts, and mold spores), and allergens. Ultrasound treatment increased the reduction of bacteria and yeast by 1 to 2 log CFU under the most favorable conditions compared with water or water-detergent controls. The effect was dependent on the type of belt material, the power applied, the exposure time, and the distance between the probe and the belt coupon. Generally, dried microorganisms were more easily removed than biofilms. The effect on mold spores was variable and appeared to be species and material dependent. Spiked allergens were also efficiently removed by using ultrasound. The results in this study pave the way for new cleaning designs for flat conveyor belts, with possibilities for savings of water, detergent, and energy consumption.

  5. Detailed analysis of charge transport in amorphous organic thin layer by multiscale simulation without any adjustable parameters

    OpenAIRE

    Uratani, Hiroki; Kubo, Shosei; Shizu, Katsuyuki; Suzuki, Furitsu; Fukushima, Tatsuya; Kaji, Hironori

    2016-01-01

    Hopping-type charge transport in an amorphous thin layer composed of organic molecules is simulated by the combined use of molecular dynamics, quantum chemical, and Monte Carlo calculations. By explicitly considering the molecular structure and the disordered intermolecular packing, we reasonably reproduce the experimental hole and electron mobilities and their applied electric field dependence (Poole-Frenkel behaviour) without using any adjustable parameters. We find that the distribution of...

  6. Amino Acid Composition, Urease Activity and Trypsin Inhibitor Activity after Toasting of Soybean in Thick and Thin Layer

    OpenAIRE

    Tajana Krička; Vanja Jurišić; Neven Voća; Duška Ćurić; Tea Brlek Savić; Ana Matin

    2009-01-01

    The objective of this study was to determine amino acid content, urease activity and trypsin inhibitor activity in soybean grain for polygastric animals’ feed aft er toasting with the aim to introduce thick layer in toasting technology. Hence, soybean was toasted both in thick and thin layer at 130 oC during 10 minutes. In order to properly monitor the technological process of soybean thermal processing, it was necessary to study crude protein content, urease activity, trypsin inhibitor activ...

  7. Diurnal changes of photosynthesis and growth of Arthrospira platensis cultured in a thin-layer cascade and an open pond

    Czech Academy of Sciences Publication Activity Database

    Benavides, A.M.S.; Ranglová, Karolína; Malapascua, José R.; Masojídek, Jiří; Torzillo, G.

    2017-01-01

    Roč. 28, DEC (2017), s. 48-56 ISSN 2211-9264 R&D Projects: GA MŠk(CZ) LO1416; GA MŠk EE2.3.30.0059 Grant - others:AV ČR(CZ) CNR-16-29 Program:Bilaterální spolupráce Institutional support: RVO:61388971 Keywords : Arthrospira platensis * Pond * Thin-layer cascade Subject RIV: EE - Microbiology, Virology Impact factor: 3.994, year: 2016

  8. Investigation into the temporal stability of aqueous standard solutions of psilocin and psilocybin using high performance liquid chromatography.

    Science.gov (United States)

    Anastos, N; Barnett, N W; Pfeffer, F M; Lewis, S W

    2006-01-01

    This paper reports an investigation into the temporal stability of aqueous solutions of psilocin and psilocybin reference drug standards over a period of fourteen days. This study was performed using high performance liquid chromatography utilising a (95:5% v/v) methanol: 10 mM ammonium formate, pH 3.5 mobile phase and absorption detection at 269 nm. It was found that the exclusion of light significantly prolonged the useful life of standards, with aqueous solutions of both psilocin and psilocybin being stable over a period of seven days.

  9. Determine equilibrium dissociation constant of drug-membrane receptor affinity using the cell membrane chromatography relative standard method.

    Science.gov (United States)

    Ma, Weina; Yang, Liu; Lv, Yanni; Fu, Jia; Zhang, Yanmin; He, Langchong

    2017-06-23

    The equilibrium dissociation constant (KD) of drug-membrane receptor affinity is the basic parameter that reflects the strength of interaction. The cell membrane chromatography (CMC) method is an effective technique to study the characteristics of drug-membrane receptor affinity. In this study, the KD value of CMC relative standard method for the determination of drug-membrane receptor affinity was established to analyze the relative KD values of drugs binding to the membrane receptors (Epidermal growth factor receptor and angiotensin II receptor). The KD values obtained by the CMC relative standard method had a strong correlation with those obtained by the frontal analysis method. Additionally, the KD values obtained by CMC relative standard method correlated with pharmacological activity of the drug being evaluated. The CMC relative standard method is a convenient and effective method to evaluate drug-membrane receptor affinity. Copyright © 2017 Elsevier B.V. All rights reserved.

  10. Comparison of standard- and nano-flow liquid chromatography platforms for MRM-based quantitation of putative plasma biomarker proteins.

    Science.gov (United States)

    Percy, Andrew J; Chambers, Andrew G; Yang, Juncong; Domanski, Dominik; Borchers, Christoph H

    2012-09-01

    The analytical performance of a standard-flow ultra-high-performance liquid chromatography (UHPLC) and a nano-flow high-performance liquid chromatography (HPLC) system, interfaced to the same state-of-the-art triple-quadrupole mass spectrometer, were compared for the multiple reaction monitoring (MRM)-mass spectrometry (MS)-based quantitation of a panel of 48 high-to-moderate-abundance cardiovascular disease-related plasma proteins. After optimization of the MRM transitions for sensitivity and testing for chemical interference, the optimum sensitivity, loading capacity, gradient, and retention-time reproducibilities were determined. We previously demonstrated the increased robustness of the standard-flow platform, but we expected that the standard-flow platform would have an overall lower sensitivity. This study was designed to determine if this decreased sensitivity could be compensated for by increased sample loading. Significantly fewer interferences with the MRM transitions were found for the standard-flow platform than for the nano-flow platform (2 out of 103 transitions compared with 42 out of 103 transitions, respectively), which demonstrates the importance of interference-testing when nano-flow systems are used. Using only interference-free transitions, 36 replicate LC/MRM-MS analyses resulted in equal signal reproducibilities between the two platforms (9.3 % coefficient of variation (CV) for 88 peptide targets), with superior retention-time precision for the standard-flow platform (0.13 vs. 6.1 % CV). Surprisingly, for 41 of the 81 proteotypic peptides in the final assay, the standard-flow platform was more sensitive while for 9 of 81 the nano-flow platform was more sensitive. For these 81 peptides, there was a good correlation between the two sets of results (R(2) = 0.98, slope = 0.97). Overall, the standard-flow platform had superior performance metrics for most peptides, and is a good choice if sufficient sample is available.

  11. Utility of thin-layer preparations in the endometrial cytology: evaluation of benign endometrial lesions.

    Science.gov (United States)

    Norimatsu, Yoshiaki; Kouda, Hiromi; Kobayashi, Tadao K; Moriya, Takuya; Yanoh, Kenji; Tsukayama, Choutatsu; Miyake, Yasuyuki; Ohno, Eiji

    2008-04-01

    The purpose of the current study was to examine the use of thin-layer cytologic (TLC) preparation compared to conventional cytologic preparation (CCP) in the normal endometrium (proliferative, secretory, atrophic) and endometrial glandular and stromal breakdown (EGBD). During a 6-month period, we compiled 158 cases by collecting a direct endometrial sample using the Uterobrush. The material comprised 40 cases of proliferative endometrium, 42 cases of secretory endometrium, 46 cases of atrophic endometrium, and 30 cases of EGBD. The following points were investigated: (1) number of endometrial epithelial cell clumps; (2) presence of TLC > CCP cases on number of epithelial cell clumps; (3) number of condensed cluster of stromal cells; (4) presence of TLC > CCP cases on number of condensed cluster of stromal cells; (5) presence of metaplastic clumps with irregular protrusion-containing condensed stromal cluster; (6) presence of a clear background; (7) presence of blood vessel in TLC; (8) presence of blood vessel of length more than diameter of a field in object x20 glasses in TLC. (1) In all phases, the number of epithelial cell clumps per a unit area of a preparation of TLC is greater than in CCP. (2) Cells (condensed cluster of stromal cells and metaplastic clumps with irregular protrusion-containing condensed stromal cluster) of useful and adequate numbers for a diagnosis of EGBD were observed in TLC. (3) In all phases, TLC was significantly higher than CCP on the appearance of a clear background. (4) The proliferative endometrium and secretory endometrium were highly significant in comparison with atrophic endometrium and EGBD, respectively, in terms of the occurrence of a blood vessel of length more than diameter of a field in object x20 glasses. Although the preparation area of TLC is smaller than that of CCP, the preparation has a clean background so that an accurate report on the patient's condition is possible. Therefore, TLC preparation is a useful tool for

  12. Simultaneous Inversion of Thickness and Ultrasonic Longitudinal Velocity for Thin Layered Structure Based on Ultrasonic Reflection Coefficient Amplitude Spectrum Matching Analysis

    OpenAIRE

    Zhang, Wei; MA Zhi-yuan; He, Li-Hua; GAO, Jian-ying; Luo, Wen; Lin, Li; LEI Ming-kai

    2016-01-01

    For the overlapped signal and unknown longitudinal velocity leading to difficulty in measuring the thickness of thin layers, a method based on ultrasonic reflection coefficient amplitude spectrum (URCAS) matching analysis technique was proposed to characterize thickness and ultrasonic longitudinal velocity of thin layered structure simultaneously. An inverse algorithm based on the correlation coefficient method was introduced. The thickness and velocity were then determined by matching the th...

  13. Biological responses to sediment remediation based on thin layer placement near a former pulp mill in Ward Cove, AK (USA).

    Science.gov (United States)

    Becker, D Scott; Sexton, Jane E; Jacobs, Lucinda A; Hogarty, Barry; Keeley, Karen

    2009-07-01

    In 2001, 28 acres of the bottom of Ward Cove, AK (USA) were remediated using thin layer placement, to enhance the natural recovery of contaminated sediments. The remediated areas were part of an 80-acre area of concern identified offshore from the site of a former sulfite pulp mill. The primary chemicals of concern were those commonly associated with organic enrichment near pulp mills: ammonia and 4-methylphenol. The primary remedial objectives were to reduce the toxicity of the contaminated sediments and to stimulate colonization of the remediated areas by benthic macroinvertebrates. In 2004, the initial monitoring event for the remediated areas was conducted, and included evaluations of physical/chemical sediment variables (i.e., total organic carbon, grain size distribution, ammonia, and 4-methylphenol), sediment toxicity (i.e., using the 10-day amphipod survival test with Eohaustorius estuarius), and in situ benthic macroinvertebrate communities. Results of the monitoring event showed that conditions in the remediated areas had improved considerably in the 3 years since thin layer placement had occurred. At most stations, concentrations of both ammonia and 4-methylphenol were very low, and amphipod survival was >or=90%. In addition, benthic macroinvertebrates appeared to be rapidly colonizing the remediated areas, based on evaluations of several community metrics (i.e., taxa richness, diversity, and dominance), as well as key indicator species of organic enrichment and associated transitional areas (i.e., primarily the polychaetes Capitella capitata and Nephtys cornuta, and the bivalve molluscs Axinopsida serricata and Parvilucina tenuisculpta). In general, colonization was consistent with the patterns identified for areas recovering from organic enrichment on the continental shelf of southern California and elsewhere. Based on these results, thin layer placement was considered successful in enhancing the natural recovery of the remediated sediments in Ward

  14. Development and validation of a high performance thin layer chromatographic method for determination of 1, 8-Cineole in Callistemon Citrinus

    OpenAIRE

    Shaha, Archana; Salunkhe, Vijay R

    2014-01-01

    A new, simple, precise, rapid, and selective high performance thin layer chromatographic (HPTLC) method has been developed and validated for the estimation of 1, 8-cineole in volatile oil of leaves of Callistemon citrinus obtained by hydro distillation. The method was validated as per ICH guidelines and can be utilized for routine analysis. The retention factor for 1, 8-cineole was found to be 0.52. The linearity was found to be in the range of 3 μg-12 μg. The recovery obtained for 1, 8-cineo...

  15. SNOM images of X-ray radiographs at nano-scale stored in a thin layer of lithium fluoride.

    Science.gov (United States)

    Oliva, C; Ustione, A; Almaviva, S; Baldacchini, G; Bonfigli, F; Flora, F; Lai, A; Montereali, R M; Faenov, A Ya; Pikuz, T A; Francucci, M; Gaudio, P; Martellucci, S; Richetta, M; Reale, L; Cricenti, A

    2008-03-01

    In this work, we report a method to observe soft X-ray radiographs at nanoscale of various kind of samples, biological and metallic, stored in a thin layer of lithium fluoride, employing scanning near-field optical microscopy with an optical resolution that reaches 50 nm. Lithium fluoride material works as a novel image detector for X-ray nano-radiographs, due to the fact that extreme ultraviolet radiation and soft X-rays efficiently produce stable point defects emitting optically stimulated visible luminescence in a thin surface layer. The bi-dimensional distribution of the so-created defects depends on the local nanostructure of the investigated sample.

  16. Ascorbic acid surface modified TiO2-thin layers as a fully integrated analysis system for visual simultaneous detection of organophosphorus pesticides

    Science.gov (United States)

    Li, Shunxing; Liang, Wenjie; Zheng, Fengying; Lin, Xiaofeng; Cai, Jiabai

    2014-11-01

    TiO2 photocatalysis and colorimetric detection are coupled with thin layer chromatography (TLC) for the first time to develop a fully integrated analysis system. Titania@polystyrene hybrid microspheres were surface modified with ascorbic acid, denoted AA-TiO2@PS, and used as the stationary phase for TLC. Because the affinity between AA-TiO2@PS and organophosphorus pesticides (OPs) was different for different species of OPs (including chlopyrifos, malathion, parathion, parathion-methyl, and methamidophos), OPs could be separated simultaneously by the mobile phase in 12.0 min with different Rf values. After surface modification, the UV-vis wavelength response range of AA-TiO2@PS was expanded to 650 nm. Under visible-light irradiation, all of the OPs could be photodegraded to PO43- in 25.0 min. Based on the chromogenic reaction between PO43- and chromogenic agents (ammonium molybdate and ascorbic acid), OPs were quantified from color intensity images using a scanner in conjunction with image processing software. So, AA-TiO2@PS was respectively used as the stationary phase of TLC for efficient separation of OPs, as a photocatalyst for species transformation of phosphorus, and as a colorimetric probe for on-field simultaneous visual detection of OPs in natural water. Linear calibration curves for each OP ranged from 19.3 nmol P L-1 to 2.30 μmol P L-1. This integrated analysis system was simple, inexpensive, easy to operate, and sensitive.TiO2 photocatalysis and colorimetric detection are coupled with thin layer chromatography (TLC) for the first time to develop a fully integrated analysis system. Titania@polystyrene hybrid microspheres were surface modified with ascorbic acid, denoted AA-TiO2@PS, and used as the stationary phase for TLC. Because the affinity between AA-TiO2@PS and organophosphorus pesticides (OPs) was different for different species of OPs (including chlopyrifos, malathion, parathion, parathion-methyl, and methamidophos), OPs could be separated

  17. Method "Ethanol as Internal Standard" for determination of volatile compounds in alcohol products by gas chromatography in daily practice

    CERN Document Server

    Charapitsa, Siarhei V; Makhomet, Andrey A; Guguchkina, Tatiana I; Markovsky, Mikhail G; Yakuba, Yurii F; Kotov, Yurii N

    2016-01-01

    Recently proposed new method "Ethanol as Internal Standard" for determination of volatile compounds in alcohol products by gas chromatography (GC) is investigated from different sides including method testing on prepared standard solutions like cognac and brandy, different ethanol-water solutions and certified reference material CRM LGC5100 Whisky-Congeners. Analysis of obtained results of experimental study from four different laboratories shows that relative bias between the experimentally measured concentrations calculated in accordance with proposed method and the values of concentrations assigned during the preparation by gravimetric method for all analyzed compounds does not exceed 10 %. It is shown that relative response factors (RRF) between analyzed volatile compounds and ethanol do not depend on time of analysis and are constant for every model of GC. It is shown the possibility to use predetermined RRF in daily practice of testing laboratories and to implement this new method in the international s...

  18. Effect of Hot Water Blanching Time and Drying Temperature on the Thin Layer Drying Kinetics of and Anthocyanin Degradation in Black Carrot (Daucus carota L. Shreds

    Directory of Open Access Journals (Sweden)

    Umar Garba

    2015-01-01

    Full Text Available This study was conducted to investigate the eff ect of blanching treatment (98 °C for 3 and 6 min and air drying temperature of 40, 50 and 60 °C on the thin layer drying characteristics such as drying time, drying rate constant, effective moisture diffusivity and activation energy, as well as on anthocyanin content of black carrot shreds. It was observed that drying temperature aff ected the drying rate but blanching did not have an eff ect on drying time. Three thin layer drying models, i.e. Page, Lewis and Henderson-Pabis were evaluated. The goodness of these models was evaluated based on the coefficient of determination (R2, root mean square error, reduced chi square (χ2 and standard error. Page model showed the best fit to the drying data. The effective diffusivity ranges of 1.4·10–9 to 2.6·10–9 m2/s, 1.3·10–9 to 2.1·10–9 m2/s and 1.5·10–9 to 2.2·10–9 m2/s aft er 3 or 6 min of blanching and control samples respectively were calculated using Fick’s second law. The activation energy of 37.5, 26.0 and 34.6 kJ/(mol·K of the control samples and samples blanched for 3 or 6 min respectively was determined from the Arrhenius plot. The blanching treatment affected the anthocyanin content to a great extent. The anthocyanin content of (231.7±2.9 and (278.8±7.8 mg per 100 g was recorded in samples blanched for 3 and 6 min and then dried at 60 °C, and (153.0±4.3 and (247.0±5.5 mg per 100 g was recorded at 40 °C as compared to the control of (580.1±1.3 at 60 °C and (466.7±1.1 mg per 100 g at 40 °C.

  19. Enzymatic hydrolysis of nylons: quantification of the reaction rate of nylon hydrolase for thin-layered nylons.

    Science.gov (United States)

    Nagai, Keisuke; Iida, Kazuki; Shimizu, Kimiaki; Kinugasa, Ryo; Izumi, Motoki; Kato, Dai-Ichiro; Takeo, Masahiro; Mochiji, Kozo; Negoro, Seiji

    2014-10-01

    Nylon hydrolase degrades various aliphatic nylons, including nylon-6 and nylon-66. We synthesized a nylon-66 copolymer (M w = 22,900, M n = 7,400), in which a part of an adipoyl unit (32 % molar ratio) of nylon-66 was replaced with a succinyl unit by interfacial polymerization. To quantify the reaction rate of the enzymatic hydrolysis of nylons at the surface of solid polymers, we prepared a thin layer of nylons on the bottom surface of each well in a polystyrene-based micro-assay plate. The thickness of the nylon layer was monitored by imaging analysis of the photographic data. More than 99 % of the copolymer with thicknesses of 260 nm (approximately 600 layers of polymer strands) were converted to water-soluble oligomers by nylon hydrolase (3 mg enzyme ml(-1)) at 30 °C within 60 h. These results were further confirmed by TLC analysis of the reaction products and by assay of liberated amino groups in the soluble fractions. The degradation rate of the thin-layered nylon-6 was similarly analyzed. We demonstrate that this assay enables a quantitative evaluation of the reaction rate of hydrolysis at the interface between the solid and aqueous phases and a quantitative comparison of the degradability for various polyamides.

  20. High-Performance Thin-Layer Chromatographic Quantification of Rosmarinic Acid and Rutin in Abnormal Savda Munziq

    Directory of Open Access Journals (Sweden)

    S. G. Tian

    2013-01-01

    Full Text Available A high-performance thin-layer chromatographic (HPTLC method has been established for simultaneous analysis of rosmarinic acid and rutin in Abnormal Savda Munziq (ASMq. A methanol extract of ASMq was used for quantification. The compounds were separated on silica gel H thin layer plate with ethyl acetate-formic acid-acetic acid-water 15 : 1 : 1 : 1.5 (v/v as a developer, trichloroethanol as the color reagent. The plates were scanned at 365 nm. The linear calibration data of rosmarinic acid and rutin were in the range of 0.0508 to 0.2540 μg (r=0.9964, 0.2707 to 1.35354 μg (r=0.9981, respectively. The recovery rate of rosmarinic acid was 99.17% (RSD = 2.92% and rutin was 95.24% (RSD = 2.38%. The method enables rapid screening, precise, selective, and sensitive quantification for pharmaceutical analysis.

  1. Quantitative statistical analysis of standard and human blood proteins from liquid chromatography, electrospray ionization, and tandem mass spectrometry.

    Science.gov (United States)

    Bowden, Peter; Thavarajah, Thanusi; Zhu, Peihong; McDonell, Mike; Thiele, Herbert; Marshall, John G

    2012-04-06

    It will be important to determine if the parent and fragment ion intensity results of liquid chromatography, electrospray ionization and tandem mass spectrometry (LC-ESI-MS/MS) experiments have been randomly and independently sampled from a normal population for the purpose of statistical analysis by general linear models and ANOVA. The tryptic parent peptide and fragment ion m/z and intensity data in the mascot generic files from LC-ESI-MS/MS of purified standard proteins, and human blood protein fractionated by partition chromatography, were parsed into a Structured Query Language (SQL) database and were matched with protein and peptide sequences provided by the X!TANDEM algorithm. The many parent and/or fragment ion intensity values were log transformed, tested for normality, and analyzed using the generic Statistical Analysis System (SAS). Transformation of both parent and fragment intensity values by logarithmic functions yielded intensity distributions that closely approximate the log-normal distribution. ANOVA models of the transformed parent and fragment intensity values showed significant effects of treatments, proteins, and peptides, as well as parent versus fragment ion types, with a low probability of false positive results. Transformed parent and fragment intensity values were compared over all sample treatments, proteins or peptides by the Tukey-Kramer Honestly Significant Difference (HSD) test. The approach provided a complete and quantitative statistical analysis of LC-ESI-MS/MS data from human blood.

  2. Comprehensive thin layer chromatography×gas chromatography using headspace sampling modulation-A case study on fatty acid composition analysis.

    Science.gov (United States)

    Križman, Mitja; Pušar, Alenka

    2015-07-31

    The recently developed comprehensive TLC×GC technique using headspace sampling is presented. The main advantage of this approach, as demonstrated in lipid analysis, is the possibility to include a transesterification step of glycerides into fatty acid methyl ester derivatives (FAME) because no particular constraints in terms of operational time between TLC and GC are present. Besides being a relatively low-cost solution, TLC×GC by means of headspace sampling provides many benefits in terms of flexibility of separation conditions and modulation sampling width. The technique provides over two orders of magnitude of linear range with TLC sample loads of about 1mg with good reproducibility and accuracy, as demonstrated by multiple headspace extraction (MHE) tests. The technique is a viable alternative to the established but more expensive HPLC×GC technique. The useful range of TLC×GC in terms of analyte volatility can be further extended with a future development of devices based on thermal desorption. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. High performance liquid chromatography, thin layer chromatography and spectrophotometric studies on the removal of biogenic amines from some Egyptian foods using organic, inorganic and natural compounds.

    Science.gov (United States)

    Mohamed, Gehad G; El-Hameed, Azza K Abd; El-Din, A M M Nezam; El-Din, Lara A M M N

    2010-04-01

    This work has been carried out to investigate the conditions which lead to removal of the biogenic amines through the model system. Also, the main goal of this research work is trying to remove biogenic amines; histamine and tyramine, from some Egyptian foods such as tomato, strawberry, banana and mango to prevent their allergy effect. Histamine and tyramine have been affected by pyrogallol, catechol, starch, ascorbic and chlorogenic acids at different levels with different conditions. Some natural additives like glucose, spices, milk, vanillin, starch, orange juice, ascorbic and citric acids, showed an effective effect on disappearance of histamine and tyramine. By studying the effect of some additives on biogenic amines, it was found that tomato showed a decrease in histamine and tyramine concentrations by adding spices. Strawberry and banana showed a clear decrease in histamine and tyramine concentrations by treating them with ascorbic acid. Treating mango by milk led to increase of histamine level while milk with chocolate increases both histamine and tyramine concentrations.

  4. Simultaneous determination of alprazolam and fluoxetine hydrochloride in tablet formulations by high-performance column liquid chromatography and high-performance thin-layer chromatography.

    Science.gov (United States)

    Patel, Rashmin B; Patel, Mrunali R; Shankar, Madhira B; Bhatt, Kashyap K

    2009-01-01

    This paper describes validated HPLC and HPTLC methods for simultaneous determination of alprazolam (ALP) and fluoxetine hydrochloride (FXT) in pure powder and formulation. The HPLC separation was achieved on a Nucleosil C8 column (150 mm length, 4.6 mm id, 5 microm particle size) using acetonitrile-phosphate buffer pH 5.5 (45 + 55, v/v) as the mobile phase at a flow rate of 1.0 mL/min at ambient temperature. The HPTLC separation was achieved on an aluminum-backed layer of silica gel 60F254 using acetone-toluene-ammonia (6.0 + 3.5 + 0.5, v/v/v) as the mobile phase. Quantification in the HPLC method was achieved with UV detection at 230 nm over the concentration range 4-14 microg/mL for both drugs, with mean recovery of 99.95 +/- 0.38 and 99.85 +/- 0.56% for ALP and FXT, respectively. Quantification in the HPTLC method was achieved with UV detection at 230 nm over the concentration range of 400-1400 ng/spot for both drugs, with mean recovery of 99.32 +/- 0.45 and 99.78 +/- 0.81% for ALP and FXT, respectively. These methods are simple, precise, and sensitive, and they are applicable for the simultaneous determination of ALP and FXT in pure powder and formulations.

  5. Simple Detection Methods for Antinutritive Factor β-ODAP Present in Lathyrus sativus L. by High Pressure Liquid Chromatography and Thin Layer Chromatography

    Science.gov (United States)

    Ghosh, Bidisha; Mitra, Joy; Chakraborty, Saikat; Bhattacharyya, Jagannath; Chakraborty, Anirban; Sen, Soumitra Kumar; Neerathilingam, Muniasamy

    2015-01-01

    Lathyrus sativus L. (Grass pea) is the source for cheap and nutritious food choice in drought and famine susceptible zones in greater part of North India and Africa. The non-protein amino acid β-N-oxalyl-L-α,β-diaminopropionic acid (β-ODAP) has been known for decades for its potent neurotoxic effect, causing irreversible neurodegenerative disease “neurolathyrism”, present in both seed and leaf of Lathyrus sativus L. and other species in varying proportions. It is crucial to establish a rapid as well as reliable detection methodology for β-ODAP content in various Lathyrus plants. Currently available HPLC based methods involve multi-step derivatization of the sample. To overcome this, we have developed β-ODAP analysis method by HPLC without any prior derivatization. This method is statistically significant in the range of 2 to 100μg/ml and exhibited linear response with r2 > 0.99. Limit of detection and quantitation of the later method was determined to be 5.56 μg/ml and 16.86 μg/ml, respectively. In addition to this, a TLC based method has also been developed. The limit of detection of β-ODAP is 0.6μg and for its substrate, L-1,2-diaminopropionic acid is 5μg. Both HPLC and TLC methods were validated by conducting in-vitro bioconversion test to detect the presence of biocatalyst in plant extract. This method is economical, rapid and simple. PMID:26524073

  6. Quantification of phenol in soil using solid-phase microextraction, gas chromatography-mass spectrometry and standard addition

    Directory of Open Access Journals (Sweden)

    Saltanat Yegemova

    2015-12-01

    Full Text Available Phenol is a toxic environmental pollutant possessing carcinogenic and mutagenic properties. Determination of phenol in soil by certified methods requires long and laborious sample preparation. Solid-phase microextraction (SPME allows much simpler and faster determination of pollutants in soils. However, method accuracy is limited by the problem of effective matrix effect control. The aim of this study was to develop a rapid and inexpensive method for the quantitative determination of phenol in soil using SPME, gas chromatography-mass spectrometry and standard addition. Extraction temperature 80°C provides the lowest relative standard deviation being 2.1 and 4.6% for aqueous and soil samples, respectively. Soil equilibration time after addition of phenol standard at 80°C should take at least 6 h. The developed method was successfully tested on model and real soil samples having phenol concentrations 0.44 and 0.059 mg/kg, respectively. Coefficients of linear approximation of calibration dependences were higher than 0.97. Method detection limit depends on the affinity of matrix to analyte and is lower than 10 µg/kg.

  7. Detailed analysis of charge transport in amorphous organic thin layer by multiscale simulation without any adjustable parameters

    Science.gov (United States)

    Uratani, Hiroki; Kubo, Shosei; Shizu, Katsuyuki; Suzuki, Furitsu; Fukushima, Tatsuya; Kaji, Hironori

    2016-12-01

    Hopping-type charge transport in an amorphous thin layer composed of organic molecules is simulated by the combined use of molecular dynamics, quantum chemical, and Monte Carlo calculations. By explicitly considering the molecular structure and the disordered intermolecular packing, we reasonably reproduce the experimental hole and electron mobilities and their applied electric field dependence (Poole-Frenkel behaviour) without using any adjustable parameters. We find that the distribution of the density-of-states originating from the amorphous nature has a significant impact on both the mobilities and Poole-Frenkel behaviour. Detailed analysis is also provided to reveal the molecular-level origin of the charge transport, including the origin of Poole-Frenkel behaviour.

  8. Development and validation of a high performance thin layer chromatographic method for determination of 1, 8-Cineole in Callistemon Citrinus.

    Science.gov (United States)

    Shaha, Archana; Salunkhe, Vijay R

    2014-04-01

    A new, simple, precise, rapid, and selective high performance thin layer chromatographic (HPTLC) method has been developed and validated for the estimation of 1, 8-cineole in volatile oil of leaves of Callistemon Citrinus obtained by hydro distillation. The method was validated as per ICH guidelines and can be utilized for routine analysis. The retention factor for 1, 8-cineole was found to be 0.52. The linearity was found to be in the range of 3 μg-12 μg. The recovery obtained for 1, 8-cineole was 98%, which is satisfactory. The result obtained in validation indicate the accuracy, reproducibility, and reliability of the developed HPTLC method for determination of 1, 8-cineole.

  9. Fabrication of hydroxyapatite ultra-thin layer on gold surface and its application for quartz crystal microbalance technique.

    Science.gov (United States)

    Monkawa, Akira; Ikoma, Toshiyuki; Yunoki, Shunji; Yoshioka, Tomohiko; Tanaka, Junzo; Chakarov, Dinko; Kasemo, Bengt

    2006-11-01

    We present a method for coating gold quartz crystal microbalance with dissipation (QCM-D) sensor with ultra-thin layer of hydroxyapatite nanocrystals evenly covering and tightly bound to the surface. The hydroxyapatite layer shows a plate-like morphology and less than 20 nm in thickness. The hydroxyapatite sensor operated in liquid with high stability and sensitivity. The in-situ adsorption mechanism and conformational change of fibrinogen on gold, titanium and hydroxyapatite surfaces were investigated by QCM-D technique and Fourier-transform infrared spectroscopy. The change of secondary structures of fibrinogen adsorbed on the surfaces depended on the adsorbed amounts of protein. The secondary structure of fibrinogen adsorbed on the surfaces changes with increasing coverage. This is explained by repulsion among fibrinogens, affecting water structure and thus the strength of fibrinogen interactions on the surface. The study indicates that the hydroxyapatite sensor is applicable for qualitative and conformational analysis of protein adsorption.

  10. Properties of different thin-layer LiF:Mg,Cu,P TL detectors for beta dosimetry

    DEFF Research Database (Denmark)

    Bilski, P.; Budzanowski, M.; Olko, P.

    1996-01-01

    Dosimetric properties of two different types of thin TL detectors, designed to measure personal doses at a depth of 7 mg.cm(-2) in tissue, have been compared. At Riso National Laboratory detectors were prepared by fixing LiF:Mg,Cu,P GR-200 thin detectors to 0.7 mm thick Al pieces. At the Institute...... of Nuclear Physics, a thin layer of LiF:Mg,Cup phosphor of effective thickness 8.5 mg.cm(-2) was sintered to a base of undoped LiF. Beta energy and angular response, detection threshold, stability, etc. were investigated for the two detector types. Results show that both detectors possess good energy...... characteristic and that their sensitivity is sufficient to measure doses below 100 mu Gy reliably. Hence, they are suitable for practical applications in extremity dosimetry....

  11. HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHIC DETERMINATION OF CAFFEIC ACID AND ROSMARINIC ACID FROM THE LEAVES OF Orthosiphon stamineus

    Directory of Open Access Journals (Sweden)

    M. Amzad Hossain

    2010-06-01

    Full Text Available This paper presents the studies performed on extraction of Orthosiphon stamineus, Benth by using different solvent for the identification and quantification of the caffeic acid derivatives such as caffeic acid  and rosmarinic acid which confers to the leaves of this plant with remarkable pharmaceutical properties. High performance thin-layer chromatographic (HPTLC allows the identification and the quantification of more than 20 samples in the same chromatographic run. The analysis of the samples requires 15-30 min compared with more than 2 h using a typical HPLC method. Using the techniques of the HPTLC and the UV-VIS spectra we have found that the extraction of this herb plant contain, the caffeic acid and rosmarinic acid ranging between 0.029% up to 0.506% and up to 0.24% to 2.24% respectively.     Keywords: Caffice acid derivatives, quantification, Malaysian Orthosiphon stamineus, HPTLC

  12. Highly efficient decomposition of Remazol Brilliant Blue R using tubular reactor coated with thin layer of PdO.

    Science.gov (United States)

    Javaid, Rahat; Qazi, Umair Yaqub; Kawasaki, Shin-Ichiro

    2016-09-15

    In this work, we propose a novel approach to dye decomposition under subcritical water conditions using a continuous-flow tubular reactor coated with thin layer of PdO as a catalyst. Remazole Brilliant Blue R was used as an example of synthetic dyes. Hydrogen peroxide was used as an environmental-friendly oxidant as it leaves no residues after treatment. The effect of temperature, pressure and dye concentration on total organic carbon (TOC) removal were studied. 99.9% of TOC removal was achieved at 300 °C and 10 MPa pressure within a short residence time of 3.2 s. This method provided an efficient and rapid process that has a potential for treating a wide range of textile wastewaters. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Thin-layer agar (TL7H11 for rapid isolation of Mycobacterium tuberculosis in sputum specimens

    Directory of Open Access Journals (Sweden)

    Habiba Binte Alam

    2016-08-01

    Full Text Available Background: Tuberculosis (TB remains one of the major causes of death from a single infectious agent worldwide. The early detection of new cases of pulmonary tuberculosis is an important goal in tuberculosis control program.Objective: 1n this study, thin layer agar (TLA culture was compared with Lowenstein-Jensen (LJ culture for rapid detection of pulmonary tuberculosis. Methods: It was a cross sectional study conducted in National Tuberculosis Reference Labora­tory (NTRL of National Institute of Disease of Chest and Hospital (NIDCH, Dhaka, from July 2010 to June 2011. A total of 100 sputum smear positive for acid fast bacilli (AFB by Z-N staining, pulmonary tuberculosis patients were included in this study. Samples were processed by modified Petroff method and then cultured on thin layer 7H11(TL7H11 plates and L-J tubes. TL7H11 plates were observed microscopically for rnicrocolony growth once a week for 6 weeks, and L-J tubes were observed once a week for 8 weeks. Results: The recovery rates of mycobacteria on only TLA, only LJ and on both media were 90%, 97% and 88% respectively. Overall positivity was 99% in both L-J and TLA media. Mean time for detection of mycobacteria on TLA was 9.04±1.66 days compared to 21.78±6.19 days on L-J media. The rate of contamination was higher (6% in L-J media than in TLA media (4%. Conclusion: The TL7H11 media can be used as an alternative to the Lowenstein-Jensen medium for early isolation of mycobacteria in resource constrained settings.

  14. Experimental study of water desorption isotherms and thin-layer convective drying kinetics of bay laurel leaves

    Science.gov (United States)

    Ghnimi, Thouraya; Hassini, Lamine; Bagane, Mohamed

    2016-12-01

    The aim of this work is to determine the desorption isotherms and the drying kinetics of bay laurel leaves ( Laurus Nobilis L.). The desorption isotherms were performed at three temperature levels: 50, 60 and 70 °C and at water activity ranging from 0.057 to 0.88 using the statistic gravimetric method. Five sorption models were used to fit desorption experimental isotherm data. It was found that Kuhn model offers the best fitting of experimental moisture isotherms in the mentioned investigated ranges of temperature and water activity. The Net isosteric heat of water desorption was evaluated using The Clausius-Clapeyron equation and was then best correlated to equilibrium moisture content by the empirical Tsami's equation. Thin layer convective drying curves of bay laurel leaves were obtained for temperatures of 45, 50, 60 and 70 °C, relative humidity of 5, 15, 30 and 45 % and air velocities of 1, 1.5 and 2 m/s. A non linear regression procedure of Levenberg-Marquardt was used to fit drying curves with five semi empirical mathematical models available in the literature, The R2 and χ2 were used to evaluate the goodness of fit of models to data. Based on the experimental drying curves the drying characteristic curve (DCC) has been established and fitted with a third degree polynomial function. It was found that the Midilli Kucuk model was the best semi-empirical model describing thin layer drying kinetics of bay laurel leaves. The bay laurel leaves effective moisture diffusivity and activation energy were also identified.

  15. Standardization method for measurement of hydroxyurea by Ultra High Efficiency Liquid Chromatography in plasma of patients with sickle cell disease

    Directory of Open Access Journals (Sweden)

    Darcielle Bruna Dias Elias

    2014-09-01

    Full Text Available Sickle cell anemia (SCA is a recessively inherited disease characterized by chronic hemolytic anemia, chronic inflammation, and acute episodes of hemolysis. Hydroxyurea (HU is widely used to increase the levels of fetal hemoglobin (HbF. The objective of this study was to standardize and validate a method for the quantification of HU in human plasma by using ultra high performance liquid chromatography (UPLC in order to determine the plasma HU levels in adult patients with SCA who had been treated with HU. We used an analytical reverse phase column (Nucleosil C18 with a mobile phase consisting of acetonitrile/water (16.7/83.3. The retention times of HU, urea, and methylurea were 6.7, 7.7, and 11.4 min, respectively. All parameters of the validation process were defined. To determine the precision and accuracy of quality controls, HU in plasma was used at concentrations of 100, 740, and 1600 µM, with methylurea as the internal standard. Linearity was assessed in the range of 50-1600 µM HU in plasma, obtaining a correlation coefficient of 0.99. The method was accurate and precise and can be used for the quantitative determination of HU for therapeutic monitoring of patients with SCA treated with HU.

  16. Determination of avermectins by the internal standard recovery correction - high performance liquid chromatography - quantitative Nuclear Magnetic Resonance method.

    Science.gov (United States)

    Zhang, Wei; Huang, Ting; Li, Hongmei; Dai, Xinhua; Quan, Can; He, Yajuan

    2017-09-01

    Quantitative Nuclear Magnetic Resonance (qNMR) is widely used to determine the purity of organic compounds. For the compounds with lower purity especially molecular weight more than 500, qNMR is at risk of error for the purity, because the impurity peaks are likely to be incompletely separated from the peak of major component. In this study, an offline ISRC-HPLC-qNMR (internal standard recovery correction - high performance liquid chromatography - qNMR) was developed to overcome this problem. It is accurate by excluding the influence of impurity; it is low-cost by using common mobile phase; and it extends the applicable scope of qNMR. In this method, a mix solution of the sample and an internal standard was separated by HPLC with common mobile phases, and only the eluents of the analyte and the internal standard were collected in the same tube. After evaporation and re-dissolution, it was determined by qNMR. A recovery correction factor was determined by comparison of the solutions before and after these procedures. After correction, the mass fraction of analyte was constant and it was accurate and precise, even though the sample loss varied during these procedures, or even in bad resolution of HPLC. Avermectin B1a with the purity of ~93% and the molecular weight of 873 was analyzed. Moreover, the homologues of avermectin B1a were determined based on the identification and quantitative analysis by tandem mass spectrometry and HPLC, and the results were consistent with the results of traditional mass balance method. The result showed that the method could be widely used for the organic compounds, and could further promote qNMR to become a primary method in the international metrological systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Monofluorinated analogues of polychlorinated biphenyls (F-PCBs) - standards for analysis. Retention behaviour in gas chromatography and MS characteristics

    Energy Technology Data Exchange (ETDEWEB)

    Johansen, J.E.; Liu, H. [CHIRON, Trondheim (Norway); Luthe, G. [NTNU, Trondheim (Norway); Leonards, P. [RIVO, Ijmuiden (Netherlands)

    2004-09-15

    Polychlorinated biphenyls (PCBs) have been the subject of a broad range of studies and investigations, because they are persistent organic pollutants (POPs). There is a concern about the health effects of PCB exposure. PCBs are structurally similar to polychlorinated dibenzodioxines (PCDDs) and polychlorinated dibenzofuranes (PCDFs) as well as to polybrominated dibenzoethers (PBDEs). Their abundance as pollutants stems from their worldwide manufacture as heavy-used industrial chemicals. The overwhelming problem with PCBs is their continuing environmental impact; their persistence, and widespread prior use has caused global contamination of soil, rivers and other waterways that can affect our food and water supplies. The high lipophilicity causes accumulation in body lipids and liver organs, and subsequent bioaccumulation in the food chain. Therefore, they have to be determined very frequently at the trace level in, e.g. water, food, sediment and soil. The sample preparation and final determination may well lead to systematic and non-systematic (random) errors. It is generally accepted that the accurate determination of micro contaminants in such complex mixtures requires the use of external or, preferably, internal standards (ISs). The benefit of using ISs with physico-chemical properties similar to those of the target compounds, is that both types of errors will be minimized. While preliminary work on monofluorinated polycyclic aromatic hydrocarbons (F-PAHs) as ISs in gas chromatography (GC) was very promising, we recently synthesized a series of monofluorinated PCBs (F-PCBs). We found that they are a very promising set of internal standards for trace-level analysis of PCBs and are alternatives to {sup 13}C-labelled analogues. In the present study, we focused attention on the retention behavior of F-PCBs in GC, and MS characteristics, with the intention to use them as calibration standards for GC-MS and electron capture detection (GCECD).

  18. Intact-protein trapping columns for proteomic analysis in capillary high-performance liquid chromatography.

    Science.gov (United States)

    Guan, Xia; Yan, Guoquan; Gao, Mingxia; Hong, Guangfeng; Deng, Chunhui; Zhang, Xiangmin

    2010-10-29

    A new type of monolithic trapping columns with high mechanical strength was prepared by thin-layer sol-gel coating method and applied to trapping intact proteins for on-line capillary liquid chromatography. Monolithic trapping columns were fabricated by entrapping C8 reversed-phase particles into the capillary columns through a sol-gel network, which was formed by hydrolysis and polycondensation of methyltriethoxysilane. Hundreds times of trapping/untrapping for intact proteins were carried out. The trapping columns showed long-term stability up to 300 bar. Recovery, loading capacity and reproducibility of trapping columns were evaluated using four proteins. The recovery of four protein mixtures for the C8 monolithic trapping columns was 99.3% on average. The loading capacity of 5 mm × 320 μm i.d. C8 trapping columns for the protein mixtures was 30 μg. Day-to-day relative standard deviation (RSD) values for recoveries of protein mixtures on the same C8 trapping column ranged from 2.34 to 5.87%, column-to-column RSD values were from 3.01 to 6.81%. The C8 trapping columns were used to trap normal mouse liver intact proteins in a capillary liquid chromatography system. Results demonstrated high efficiency of the monolithic trapping columns for trapping intact proteins for proteomic analysis in on-line capillary liquid chromatography system. Copyright © 2010 Elsevier B.V. All rights reserved.

  19. Antidiarrheal potential of standardized extract of Rhododendron arboreum Smith flowers in experimental animals.

    Science.gov (United States)

    Verma, Neeraj; Singh, Anil P; Gupta, Amresh; Sahu, P K; Rao, Ch V

    2011-11-01

    To investigate standardized ethyl acetate fraction of Rhododendron arboreum (EFRA) flowers for antidiarrheal activity in experimental animals. A simple sensitive high performance thin layer chromatography (HPTLC) method was used for the determination of hyperin in EFRA. The standardized fraction was investigated for castor oil, magnesium sulfate-induced diarrhea, measurement of gastrointestinal transit using charcoal and castor oil-induced enteropooling. The concentration of hyperin in flowers of R. arboreum was found to be 0.148% by HPTLC. Oral administration of EFRA at 100, 200 and 400 mg/kg exhibited dose-dependent and significant (Parboreum flowers has potent antidiarrheal activity thus justifying its traditional use in diarrhea and have great potential as a source for natural health products.

  20. Thin-layer effects in glaciological seismic amplitude-versus-angle (AVA analysis: implications for characterising a subglacial till unit, Russell Glacier, West Greenland

    Directory of Open Access Journals (Sweden)

    A. D. Booth

    2012-08-01

    Full Text Available Seismic amplitude-versus-angle (AVA methods are a powerful means of quantifying the physical properties of subglacial material, but serious interpretative errors can arise when AVA is measured over a thinly-layered substrate. A substrate layer with a thickness less than 1/4 of the seismic wavelength, λ, is considered "thin", and reflections from its bounding interfaces superpose and appear in seismic data as a single reflection event. AVA interpretation of subglacial till can be vulnerable to such thin-layer effects, since a lodged (non-deforming till can be overlain by a thin (metre-scale cap of dilatant (deforming till. We assess the potential for misinterpretation by simulating seismic data for a stratified subglacial till unit, with an upper dilatant layer between 0.1–5.0 m thick (λ / 120 to > λ / 4, with λ = 12 m. For dilatant layers less than λ / 6 thick, conventional AVA analysis yields acoustic impedance and Poisson's ratio that indicate contradictory water saturation. A thin-layer interpretation strategy is proposed, that accurately characterises the model properties of the till unit. The method is applied to example seismic AVA data from Russell Glacier, West Greenland, in which characteristics of thin-layer responses are evident. A subglacial till deposit is interpreted, having lodged till (acoustic impedance = 4.26±0.59 × 106 kg m−2 s−1 underlying a water-saturated dilatant till layer (thickness < 2 m, Poisson's ratio ~ 0.5. Since thin-layer considerations offer a greater degree of complexity in an AVA interpretation, and potentially avoid misinterpretations, they are a valuable aspect of quantitative seismic analysis, particularly for characterising till units.

  1. Development of a Postcolumn Infused-Internal Standard Liquid Chromatography Mass Spectrometry Method for Quantitative Metabolomics Studies.

    Science.gov (United States)

    Liao, Hsiao-Wei; Chen, Guan-Yuan; Wu, Ming-Shiang; Liao, Wei-Chih; Lin, Ching-Hung; Kuo, Ching-Hua

    2017-02-03

    Quantitative metabolomics has become much more important in clinical research in recent years. Individual differences in matrix effects (MEs) and the injection order effect are two major factors that reduce the quantification accuracy in liquid chromatography-electrospray ionization-mass spectrometry-based (LC-ESI-MS) metabolomics studies. This study proposed a postcolumn infused-internal standard (PCI-IS) combined with a matrix normalization factor (MNF) strategy to improve the analytical accuracy of quantitative metabolomics. The PCI-IS combined with the MNF method was applied for a targeted metabolomics study of amino acids (AAs). D8-Phenylalanine was used as the PCI-IS, and it was postcolumn-infused into the ESI interface for calibration purposes. The MNF was used to bridge the AA response in a standard solution with the plasma samples. The MEs caused signal changes that were corrected by dividing the AA signal intensities by the PCI-IS intensities after adjustment with the MNF. After the method validation, we evaluated the method applicability for breast cancer research using 100 plasma samples. The quantification results revealed that the 11 tested AAs exhibit an accuracy between 88.2 and 110.7%. The principal component analysis score plot revealed that the injection order effect can be successfully removed, and most of the within-group variation of the tested AAs decreased after the PCI-IS correction. Finally, targeted metabolomics studies on the AAs showed that tryptophan was expressed more in malignant patients than in the benign group. We anticipate that a similar approach can be applied to other endogenous metabolites to facilitate quantitative metabolomics studies.

  2. Guanidinated protein internal standard for immunoaffinity-liquid chromatography/tandem mass spectrometry quantitation of protein therapeutics.

    Science.gov (United States)

    Yang, Wenchu; Kernstock, Robert; Simmons, Neal; Alak, Ala

    2014-07-15

    A protein internal standard (IS) is essential and superior to a peptide IS to achieve reproducible results in the quantitation of protein therapeutics using immunoaffinity-liquid chromatography/tandem mass spectrometry (LC/MS/MS). Guanidination has been used as a protein post-modification technique for more than half a century. A decade ago, the modification was applied to lysine-ending peptides to enhance their MALDI responses and peptide sequencing coverage. However, rarely has tryptic digestion of guanidinated proteins been investigated, likely due to the early conclusion that trypsin did not hydrolyze peptide bonds involving homoarginine in guanidinated proteins. In this study, the opposite was observed. Guanidinated lysine residues of proteins did not hinder the access of trypsin allowing for proteolytic digestion. Based on this observation, a new concept of internal standard, named Guanidinated Protein Internal Standard (GP-IS), was proposed for LC/MS/MS quantitation of protein therapeutics. The GP-IS is prepared by treating a portion of the therapeutic protein (analyte) with guanidine to convert arginine residues in the protein into homoarginine residues. After tryptic digestion, the GP-IS produces a series of homoarginine-ending peptides plus another series of arginine-ending peptides. One of the homoarginine-ending peptides, which corresponds to the analyte surrogate (lysine-ending) peptide, was chosen as a peptide internal standard (GP-PIS) for LC/MS/MS quantitation. Using this GP-IS approach, a sensitive and robust immunoaffinity-LC/MS/MS assay was developed and fully validated with a linearity range from 10 to 1000 ng/mL using 200 μL of human serum for the quantitation of an Astellas protein drug in clinical development. The proposed strategy allows LC/MS/MS to play an ever-increasing role in bioanalytical support for protein therapeutics development because of its capability of completely tracking all variations from the beginning to the end of sample

  3. The November 2002 Pyroclastic Flows at El Reventador, Ecuador: Computer Simulations Using the TITAN Thin-layer Code

    Science.gov (United States)

    Burkett, B.; Sheridan, M. F.

    2007-05-01

    On November 3, 2002, El Reventador volcano, located on the eastern flank of the Ecuadorian Andes, produced a sudden, violent eruption culminating in a 17km high column containing mostly steam and ash. Explosions in the initial phase created a summit crater while generating four lithic-rich andesitic pyroclastic flows. The longest of these flows traveled ESE out of the breached caldera, obliquely overriding the 200-400m southern caldera wall, reaching the Quijos River 8km distant. This flow crossed the major oil pipelines of Ecuador, displacing a pressurized crude oil pipeline more than 100m. The flows contained mostly lithic fragments with only minor juvenile pumice. The accompanying ash-cloud surge deposited a thin layer on top of the PF deposit, indicating an abundance of gas within the flow. The eruption came with practically no warning and yet had a large socio- economic impact for Ecuador. While the flows themselves resulted in no loss of life, the lack of significant precursor activity underscores the necessity for detailed pre-eruption knowledge of the potential hazards and risk zones around a particular volcano so as to be prepared in the event of such "surprise" eruptions. In conjunction with field mapping, computer models of volcanogenic flows can be used not only to identify risk zones but to understand the evolution of these flows. A new set of computer simulations using the TITAN (www.gmfg.buffalo.edu) thin-layer code allows a more complete exploration of important flow properties associated with this type of eruption. Realizations of this code simulate the path, extent, flow thickness, velocity, and momentum of the flows given the set of initial conditions (volume, starting location, flux hydrograph, internal friction, and basal friction). The TITAN code was used to simulate the four lithic-rich pyroclastic flows generated at the beginning of the 2002 eruption. Using field estimated volumes and starting positions of the PFs, simulations of the two

  4. Determination of Polycyclic Aromatic Hydrocarbons in Automobile Exhaust by Means of High-Performance Liquid Chromatography with Fluorescence Detection

    DEFF Research Database (Denmark)

    Nielsen, Tom

    1979-01-01

    A chromatographic method has been developed and applied to the determination of polycyclic aromatic hydrocarbons (PAHs) in particulate matter in automobile exhaust, in petrols, and in crankcase oils. The PAHs were purified from other organic compounds by thin-layer chromatography, separated by high-performance...

  5. Optimal Color Stability for White Organic Light-Emitting Diode (WOLED by Using Multiple-Ultra-Thin Layers (MUTL

    Directory of Open Access Journals (Sweden)

    Kan-Lin Chen

    2013-01-01

    Full Text Available The work demonstrates the improvement of color stability for white organic light-emitting diode (WOLED. The devices were prepared by vacuum deposition on ITO-glass substrates. These guest materials of 5,6,11,12-tetraphenylnaphthacene (Rubrene were deposited in 4,4′-bis(2,2-diphenyl vinyl-1,1′-biphenyl (DPVBi, resulting in an emitting layer. Experimental results reveal that the properties in the multiple-ultra-thin layer (MUTL are better than those of the emitting layer with a single guest material, reaching the commercial white-light wavelength requirement of 400–700 nm. The function of the MUTL is as the light-emitting and trapping layer. The results show that the MUTL has excellent carrier capture effect, leading to high color stability of the device at various applied voltages. The Commissions Internationale De L’Eclairage (CIE coordinate of this device at 3~7 V is few displacement and shows a very slight variation of (0.016, 0.009. The CIE coordinates at a maximal luminance of 9980 cd/m2 are (0.34, 0.33.

  6. Parametric optimization in virtual prototyping environment of the control device for a robotic system used in thin layers deposition

    Science.gov (United States)

    Enescu (Balaş, M. L.; Alexandru, C.

    2016-08-01

    The paper deals with the optimal design of the control system for a 6-DOF robot used in thin layers deposition. The optimization is based on parametric technique, by modelling the design objective as a numerical function, and then establishing the optimal values of the design variables so that to minimize the objective function. The robotic system is a mechatronic product, which integrates the mechanical device and the controlled operating device.The mechanical device of the robot was designed in the CAD (Computer Aided Design) software CATIA, the 3D-model being then transferred to the MBS (Multi-Body Systems) environment ADAMS/View. The control system was developed in the concurrent engineering concept, through the integration with the MBS mechanical model, by using the DFC (Design for Control) software solution EASY5. The necessary angular motions in the six joints of the robot, in order to obtain the imposed trajectory of the end-effector, have been established by performing the inverse kinematic analysis. The positioning error in each joint of the robot is used as design objective, the optimization goal being to minimize the root mean square during simulation, which is a measure of the magnitude of the positioning error varying quantity.

  7. Detection of arecoline by simple high-performance thin-layer chromatographic method in Indian nontobacco pan masala.

    Science.gov (United States)

    Adhikari, Anjan; Hazra, Alok Kumar; Sur, Tapas Kumar

    2015-01-01

    Chewing the habit of blended pan masala containing areca nut with or without tobacco is a common practice in the Indian subcontinent. Arecoline, a pyridine alkaloid presence in areca nut alarmed for oral carcinogenesis and strictly prohibited in the western world. However, in India using blended pan masala is very popular among young and old individuals. In this context, we aimed to detect arecoline in Indian blended nontobacco pan masala sold in Kolkata using a simple densitometric high-performance thin-layer chromatographic (HPTLC) method and for alarming their use in common people. Eleven popularly Indian blended nontobacco pan masala were collected from the territory of Kolkata and isolated arecoline, following solvent extraction method derived for pyridine alkaloid. The quantitative analysis of arecoline was measured using automated software-based HPTLC instruments and validated the method according to International Conference on Harmonization guidelines. Arecoline was detected in all 11 blended nontobacco pan masala samples in a range of minimum 130 to maximum 415 μg/g dry samples. Arecoline is hazardous carcinogenic compound, so the use of Indian blended nontobacco pan masala should be restricted. Further, the method was found suitable for routine quantitative analysis of arecoline in areca nut containing substances.

  8. THE RAMAN SPECTROSCOPY USE FOR MONITORING OF CHANGES IN THE GLASS STRUCTURE OF THE THIN LAYERS CAUSED BY ION IMPLANTATION

    Directory of Open Access Journals (Sweden)

    Pavla Nekvindova

    2015-09-01

    Full Text Available In this paper, we have demonstrated the utility of Raman spectroscopy as a technique for the characterisation of changes in the glass structure of the thin layers caused by ion implantation. Various types of silicate glasses were implanted by Au+ ions with energy of 1.7 MeV and a fluence of 1 x 1016 ions.cm-2 to create gold nanoparticles in thin sub-surface layer of the glass. It was proved that the structure of the glass has an indisputable impact on the extent of depolymerisation of the glass network after implantation. It was shown that the degree of glass matrix depolymerisation can be described using the evaluation of Qn factors in the implanted layers from different depths. After analysis of Raman spectra, the relation between nucleation and the resulting parameters of the gold nanoparticles was put into connection with the feasibility of the glass to recover its structure during post-implantation annealing. Also the creation of new bonds in the glass network was discussed.

  9. Evaluation of the mass transfer process on thin layer drying of papaya seeds from the perspective of diffusive models

    Science.gov (United States)

    Dotto, Guilherme Luiz; Meili, Lucas; Tanabe, Eduardo Hiromitsu; Chielle, Daniel Padoin; Moreira, Marcos Flávio Pinto

    2018-02-01

    The mass transfer process that occurs in the thin layer drying of papaya seeds was studied under different conditions. The external mass transfer resistance and the dependence of effective diffusivity ( D EFF ) in relation to the moisture ratio ( \\overline{MR} ) and temperature ( T) were investigated from the perspective of diffusive models. It was verified that the effective diffusivity was affected by the moisture content and temperature. A new correlation was proposed for drying of papaya seeds in order to describe these influences. Regarding the use of diffusive models, the results showed that, at conditions of low drying rates ( T ≤ 70 °C), the external mass transfer resistance, as well as the dependence of the effective diffusivity with respect to the temperature and moisture content should be considered. At high drying rates ( T > 90 °C), the dependence of the effective diffusivity with respect to the temperature and moisture content can be neglected, but the external mass transfer resistance was still considerable in the range of air velocities used in this work.

  10. Stability indicating high performance thin layer chromatographic method for quantitation of venlafaxine in bulk and pharmaceutical dosage form

    Directory of Open Access Journals (Sweden)

    Sunil K Dubey

    2015-01-01

    Full Text Available Background: Venlafaxine (VEN is a phenethylamine bicyclic compound, chemically, 1-(2-[dimethyl amino]-1-[4-methoxy phenyl] ethyl cyclo-hexan-1ol hydrochloride. It is a antidepressant. It inhibits the reuptake of serotonin, nor adrenaline and dopamine to a lesser extent at the presynaptic membrane. Aim: A simple, rapid, precise, accurate, and economical high performance thin layer chromatographic (HPTLC method has been developed and validated for the determination of VEN both as a bulk drug and in formulation. Materials and Methods: The method uses aluminum plates precoated with silica gel 60 F254 as the stationary phase and dichloromethane:acetonitrile:N-hexane:triethylamine: 0.5:0.5:4:0.7 (v/v/v/v as mobile phase. Results: This system gave compact spots for VEN (R f = 0.46 ± 0.05. Forced degradation studies were done by subjecting VEN to acid and alkali hydrolysis, oxidation, and reduction. The peak of the degradation product was well resolved from that of the pure drug and had significant different R f values. Analysis of VEN was performed in the absorbance mode at 225 nm. The limit of detection and quantification were 12.48 and 37.81 ng/spot respectively. Conclusions: The developed method was validated and found to be simple, specific, accurate and precise and can be used for routine quality control analysis of VEN in bulk and pharmaceutical formulation.

  11. Evaluation of the mass transfer process on thin layer drying of papaya seeds from the perspective of diffusive models

    Science.gov (United States)

    Dotto, Guilherme Luiz; Meili, Lucas; Tanabe, Eduardo Hiromitsu; Chielle, Daniel Padoin; Moreira, Marcos Flávio Pinto

    2017-09-01

    The mass transfer process that occurs in the thin layer drying of papaya seeds was studied under different conditions. The external mass transfer resistance and the dependence of effective diffusivity (D EFF ) in relation to the moisture ratio ( \\overline{MR} ) and temperature (T) were investigated from the perspective of diffusive models. It was verified that the effective diffusivity was affected by the moisture content and temperature. A new correlation was proposed for drying of papaya seeds in order to describe these influences. Regarding the use of diffusive models, the results showed that, at conditions of low drying rates (T ≤ 70 °C), the external mass transfer resistance, as well as the dependence of the effective diffusivity with respect to the temperature and moisture content should be considered. At high drying rates (T > 90 °C), the dependence of the effective diffusivity with respect to the temperature and moisture content can be neglected, but the external mass transfer resistance was still considerable in the range of air velocities used in this work.

  12. Photosynthesis of Scenedesmus obliquus in outdoor open thin-layer cascade system in high and low CO2 in Belgium.

    Science.gov (United States)

    de Marchin, Thomas; Erpicum, Michel; Franck, Fabrice

    2015-12-10

    Two outdoor open thin-layer cascade systems operated as batch cultures with the alga Scenedesmus obliquus were used to compare the productivity and photosynthetic acclimations in control and CO2 supplemented cultures in relation with the outdoor light irradiance. We found that the culture productivity was limited by CO2 availability. In the CO2 supplemented culture, we obtained a productivity of up to 24gdwm(-2)day(-1) and found a photosynthetic efficiency (value based on the PAR solar radiation energy) of up to 5%. In the CO2 limited culture, we obtained a productivity of up to 10gdwm(-2)day(-1) while the photosynthetic efficiency was up to 3.3% and decreased to 2.1% when the integrated daily PAR increased. Fluorescence and oxygen evolution measurements showed that ETR and oxygen evolution light saturation curves, as well as light-dependent O2 uptake were similar in algal samples from both cultures when the CO2 limitation was removed. In contrast, we found that CO2 limitation conducted to a decreased PSII photochemical efficiency and an increased light-induced heat-dissipation in the control culture compared to the CO2 supplemented culture. These features are in line with a lower light use efficiency and may therefore contribute to the lower productivity observed in absence of CO2 supplementation in outdoor mass cultures of S. obliquus. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Surface Behavior of Rhodamin and Tartrazine on Silica-Cellulose Sol-Gel Surfaces by Thin Layer Elution

    Directory of Open Access Journals (Sweden)

    Surjani Wonorahardjo

    2016-05-01

    Full Text Available Physical and chemical interactions are the principles for different types of separation systems as the equillibrium dynamics on surface plays a key-role. Surface modification is a way for selective separation at interfaces. Moreover, synthesis of gel silica by a sol-gel method is preferred due to the homogeneity and surface feature easily controlled. Cellulose can be added in situ to modified the silica features during the process. Further application for to study interaction of rhodamin and tartrazine in its surface and their solubilities in mobile phase explains the possibility for their separation. This paper devoted to evaluate the surface behavior in term of adsorption and desorption of tartrazine and rhodamin on silica-cellulose thin layer in different mobile phase. Some carrier liquids applied such as methanol, acetone, n-hexane and chloroform. The result proves tartrazine and rhodamin is separated and have different behavior in different mobile phase. The retardation factors (Rf of the mixtures suggest complexity behavior on silica-cellulose surface.

  14. Synthesis and dielectric properties of thin-layered (La,Nd)TiO{sub 2}N perovskites

    Energy Technology Data Exchange (ETDEWEB)

    Ahchawarattaworn, J.; Thompson, Derek P. [Newcastle Univ., Newcastle upon Tyne (United Kingdom). School of Chemical Engineering and Advanced Materials; Azough, F.; Freer, R. [Manchester Univ. (United Kingdom). School of Materials

    2016-07-01

    Dielectric measurements made on thin layers of oxynitride of composition (La,Nd)TiO{sub 2}N deposited on substrates of the equivalent pure oxides gave high and variables values for the relative permittivity, and very high values of dielectric loss, showing that the samples were significantly conducting. This is believed to be due to reduction taking place during the nitridation step, the use of ammonia (by far the most convenient and effective nitriding agent for this purpose) resulting in the simultaneous production of active atomic hydrogen which easily diffuses through both the surface oxide and the simultaneously forming layer of oxynitride to give compositions of the type (La,Nd){sub 2}Ti{sup IV}{sub 2-x}Ti{sup III}{sub x}O{sub 7-x/2} and La{sub x}Nd{sub 1-x}Ti{sup 4+}{sub 1-y}Ti{sup 3+}{sub y}O2{sub -y/2}N respectively. It is well established that the presence of Ti{sup 3+} in titanium oxides and oxynitrides readily promotes conductivity. These results explain the diverse dielectric property measurements reported by previous researchers working on oxynitride materials, and show that alternative nitridation methods are needed in order to determine correct values of dielectric properties of pure oxynitride materials.

  15. Evaluation of laser-induced thin-layer removal by using shadowgraphy and laser-induced breakdown spectroscopy

    Science.gov (United States)

    Rabasović, M. S.; Šević, D.; Lukač, N.; Jezeršek, M.; Možina, J.; Gregorčič, P.

    2016-03-01

    Shadow photography and laser-induced breakdown spectroscopy (LIBS) are studied as methods for monitoring the selective removal of thin (i.e., under 100 μm) layers by laser ablation. We used a laser pulse of 5 ns and 16 mJ at 1064 nm to ablate an 18-μm-thin copper layer from the fiberglass substrate. On the basis of shadowgraphs of the laser-induced shock waves, we measured the optodynamic energy-conversion efficiency, defined as the ratio between the mechanical energy of the shock wave and the excitation-pulse energy. Our results show that this efficiency is significantly higher for the laser pulse-copper interaction than for the interaction between the excitation pulse and the substrate. LIBS was simultaneously employed in our experimental setup. The optical emission from the plasma plume was collected by using a spectrograph and recorded with a streak camera. We show that advancing of laser ablation through the copper layer and reaching of the substrate can be estimated by tracking the spectral region between 370 and 500 nm. Therefore, the presented results confirm that LIBS method enables an on-line monitoring needed for selective removal of thin layers by laser.

  16. EFFECT OF OPERATING CONDITIONS ON THIN LAYERS OF TITANIUM POSED ON STEEL 100C6 SUBSTRATES WITH PVD METHOD

    Directory of Open Access Journals (Sweden)

    R. Gheriani

    2015-08-01

    Full Text Available We proposed to prepare hard coatings based on titanium carbides by deposition of thin layers of pure Ti by sputtering method on steel substrates 100C6 of 1 %mass carbon. The samples were annealed under vacuum in the temperature range of 400 ° C to 1000 ° C, in order to activate the reaction between the two parts of the system which results the formation of carbides of Ti due to the diffusion of carbon from the substrate towards deposited  layers. We therefore note an improvement in mechanical properties such as hardness. To demonstrate the effect of deposition parameters, we have prepared two series, the first one with a high pressure of argon and remarkable energy of extracted atoms, and in the case of the second one the pressure and kinetic energy are relatively less important. The samples of series 2 show features more important: a compact structure and good mechanical properties. The reaction between thin films and substrates is studied by x-ray diffraction (XRD, scanning electron microscopy (SEM. The measurements of microhardness were performed with the Vickers method.

  17. Thin-layer heap bioleaching of copper flotation tailings containing high levels of fine grains and microbial community succession analysis

    Science.gov (United States)

    Hao, Xiao-dong; Liang, Yi-li; Yin, Hua-qun; Liu, Hong-wei; Zeng, Wei-min; Liu, Xue-duan

    2017-04-01

    Thin-layer heap bioleaching of copper flotation tailings containing high levels of fine grains was carried out by mixed cultures on a small scale over a period of 210 d. Lump ores as a framework were loaded at the bottom of the ore heap. The overall copper leaching rates of tailings and lump ores were 57.10wt% and 65.52wt%, respectively. The dynamic shifts of microbial community structures about attached microorganisms were determined using the Illumina MiSeq sequencing platform based on 16S rRNA amplification strategy. The results indicated that chemolithotrophic genera Acidithiobacillus and Leptospirillum were always detected and dominated the microbial community in the initial and middle stages of the heap bioleaching process; both genera might be responsible for improving the copper extraction. However, Thermogymnomonas and Ferroplasma increased gradually in the final stage. Moreover, the effects of various physicochemical parameters and microbial community shifts on the leaching efficiency were further investigated and these associations provided some important clues for facilitating the effective application of bioleaching.

  18. Suppression of deleterious effects of free silanols in liquid chromatography by imidazolium tetrafluoroborate ionic liquids.

    Science.gov (United States)

    Kaliszan, Roman; Marszałł, Michał Piotr; Markuszewski, Michał Jan; Baczek, Tomasz; Pernak, Juliusz

    2004-03-19

    Silica-based stationary phases are commonly used in liquid chromatography, but their surface acidity causes known problems, especially when separating basic compounds. Deleterious effects of free silanols are not fully removed by standard prevention procedures consisting in adding alkylamines or other amino quenchers to the eluents. We found that ionic liquids of the imidazolium tetrafluoroborate class, added to mobile phases at concentrations of 0.5-1.5% (v/v), blocked silanols and provided excellent thin-layer chromatographic separations of strongly basic drugs which were otherwise not eluted, even with neat acetonitrile as the mobile phase. The silanol suppressing potency of imidazolium tetrafluoroborates was demonstrated to markedly exceed that of the standard mobile phase additives, like triethylamine, dimethyloctylamine and ammonia. The proposed new mobile phase additives were also demonstrated to provide reliable lipophilicity parameters of base drug analytes as determined by gradient mode of high-performance liquid chromatography. By applying the readily available and environmentally friendly imidazolium tetrafluoroborate ionic liquids, simple and efficient means of improvement of liquid chromatographic analysis of organic bases were elaborated.

  19. Effect of Tin Electrode (Sn, Electrode Distance and Thin Layer Size of Zinc Phthalocyanine (ZnPc to Resistance Changes With Ozone Exposure

    Directory of Open Access Journals (Sweden)

    Agustina Mogi

    2018-01-01

    Full Text Available This study was aimed to determine the effect of tin electrode distances and the thickness of a thin layer of ZnPc (Zinc phtyalocyanine toward changes in resistance with ozone exposure. Tin deposition on the glass surface was conducted using spraying method. The reaction between ozone and ZnPc produces electrical properties that can be read through the resistance value of the multimeter. Based on this study, it was investigated that the smaller a distance between the electrode and the thicker deposition of ZnPc lead to the less resistance. This showed that a thin layer of the conductivity increases along with the longer exposure to ozone gas. The movement of electrons with the hole was free.

  20. Simultaneous Inversion of Thickness and Ultrasonic Longitudinal Velocity for Thin Layered Structure Based on Ultrasonic Reflection Coefficient Amplitude Spectrum Matching Analysis

    Directory of Open Access Journals (Sweden)

    ZHANG Wei

    2016-10-01

    Full Text Available For the overlapped signal and unknown longitudinal velocity leading to difficulty in measuring the thickness of thin layers, a method based on ultrasonic reflection coefficient amplitude spectrum (URCAS matching analysis technique was proposed to characterize thickness and ultrasonic longitudinal velocity of thin layered structure simultaneously. An inverse algorithm based on the correlation coefficient method was introduced. The thickness and velocity were then determined by matching the theoretical and experimental URCAS within the effective frequency band of ultrasonic probe and inversing the ultrasonic testing parameters which corresponding to the maximum correlation coefficient. Experimental validation was conducted on the radar absorbing coatings (RAC on the aluminum alloy substrates. The results show that this method can realize extraction of the ultrasonic parameters from the overlapped signal effectively, the relative errors between ultrasonic and micrometer measurement are in the range of 2.53%-3.72% for the thickness, and 2.51%-3.75% for the longitudinal velocity.

  1. Marine snow, zooplankton and thin layers: indications of a trophic link from small-scale sampling with the Video Plankton Recorder

    DEFF Research Database (Denmark)

    Möller, Klas O.; St. John, Michael; Temming, Axel

    2012-01-01

    sampling does not collect marine snow quantitatively and cannot resolve so-called thin layers in which this interaction occurs. Hence, field evidence for the importance of the marine snow−zooplankton link is scarce. Here we employed a Video Plankton Recorder (VPR) to quantify small-scale (metres) vertical...... distribution patterns of fragile marine snow aggregates and zooplankton in the Baltic Sea during late spring 2002. By using this non-invasive optical sampling technique we recorded a peak in copepod abundance (ca. 18 ind. l−1) associated with a pronounced thin layer (50 to 55 m) of marine snow (maximum...... to aggregates and demonstrating feeding behaviour, which also suggests a trophic interaction. Our observations highlight the potential significance of marine snow in marine ecosystems and its potential as a food resource for various trophic levels, from bacteria up to fish...

  2. Shear mechanical property of β-Si{sub 3}N{sub 4} nano-thin layers in the basal plane using molecular dynamics simulations

    Energy Technology Data Exchange (ETDEWEB)

    Lu, Xuefeng, E-mail: luxuefeng1979@163.com; Guo, Xin, E-mail: guoguox2008@163.com; Yin, Jianbo; Wei, Yupeng; Nan, Xueli; Dong, Qizheng; Ma, Yingxia; La, Peiqing

    2015-11-11

    Molecular dynamics simulations are performed to clarify the shear mechanical property of β-Si{sub 3}N{sub 4} nano-thin layer in the basal plane with different extreme strain rates and loading temperatures. The thin layer displays nonlinear and linear response stress–strain relationships, and fracture stresses and strains increase gradually with increasing the strain rates, which is attributed to the appearance of a great quantity of single nitrogen atom and “turtle-like” hexagon defects. With increasing loading temperature, there is a noticeable drop in both fracture stress and fracture strain. In the higher loading temperature range, the lower fracture stresses are obtained owing to the disappearance of defects mentioned above, which can be also elaborated by a combination of factors such as the appeared N{sup 6h}–Si bond breaking alone in configuration evolution and the accompanied lower total energy.

  3. Use of bergenin as an analytical marker for standardization of the polyherbal formulation containing Saxifraga ligulata.

    Science.gov (United States)

    Pushpalatha, Hulikal Basavarajaiah; Pramod, Kumar; Devanathan, Rajendran; Sundaram, Ramachandran

    2015-05-01

    Bergenin is the principle constituent of the well-known medicinal plant Saxifraga ligulata. Bergenin has anti-inflammatory, antipyretic, antiviral, immunostimulant, antihyperglycemic, and antioxidant properties. In this study, the presence of bergenin in Saxifraga ligulata and the formulations was identified using high performance thin layer chromatograpy fingerprinting technique. To develop a novel quantitative method for the estimation of bergenin using high performance liquid chromatography. The compound was separated, characterised and quantified using authentic reference standard. The method was validated per ICH guidelines for the parameters of accuracy, precision, linearity, limit of detection, limit of quantification and robustness. The method was found to be accurate, linear (r2 = 0.998) and precise (%RSD Saxifraga ligulata containing formulations.

  4. Effects of Na incorporation and plasma treatment on Bi{sub 2}S{sub 3} ultra-thin layers

    Energy Technology Data Exchange (ETDEWEB)

    Moreno-Garcia, H., E-mail: hamog@ier.unam.mx [Laboratorio de Espectroscopía, Instituto de Ciencias Físicas, Universidad Nacional Autónoma de México, Apartado Postal 48-3, 62210 Cuernavaca, Morelos (Mexico); Messina, S. [Universidad Autónoma de Nayarit, Ciudad de la Cultura “Amado Nervo” S/N, C.P. 63155 Tepic, Nayarit (Mexico); Calixto-Rodriguez, M. [Universidad Tecnológica Emiliano Zapata del Estado de Morelos, Av. Universidad Tecnológica No. 1, C.P. 62760 Emiliano Zapata, Morelos (Mexico); Martínez, H. [Laboratorio de Espectroscopía, Instituto de Ciencias Físicas, Universidad Nacional Autónoma de México, Apartado Postal 48-3, 62210 Cuernavaca, Morelos (Mexico)

    2016-04-01

    As-deposited bismuth sulfide thin films prepared by means of a chemical bath deposition were treated with argon AC plasma. In this paper, we present the results on the physical modifications which were observed when a pre-treatment, containing a solution of 1 M sodium hydroxide, was applied to the glass substrates before depositing the bismuth sulfide. The bismuth sulfide thin films were characterized by X-ray diffraction, energy dispersive X-ray spectroscopy, scanning electron microscopy, atomic force microscopy, UV–VIS, and electrical measurements. The XRD analysis demonstrated an enhancement in the crystalline properties, as well as an increment in the crystal size. The energy band gap value was calculated as 1.60 eV. Changes in photoconductivity (σ{sub p}) values were also observed due to the pre-treatment in NaOH. A value of σ{sub p} = 6.2 × 10{sup −6} (Ω cm){sup −1} was found for samples grown on substrates without pre-treatment, and a value of σ{sub p} = 0.28 (Ω cm){sup −1} for samples grown on substrates with pre-treatment. Such σ{sub p} values are optimal for the improvement of solar cells based on Bi{sub 2}S{sub 3} thin films as absorber material. - Highlights: • We report our findings about Na incorporation and plasma treatment on Bi{sub 2}S{sub 3} thin layers. • The Na pre-treatment improves the structural and electrical properties of Bi{sub 2}S{sub 3} films. • The E{sub g} value was 1.60 eV for films with pre-treatment with NaOH and treatment in Ar plasma.

  5. An optically transparent thin-layer electrochemical cell for the study of vibrational circular dichroism of chiral redox-active molecules.

    Science.gov (United States)

    Domingos, Sérgio R; Luyten, Henk; van Anrooij, Fred; Sanders, Hans J; Bakker, Bert H; Buma, Wybren J; Hartl, František; Woutersen, Sander

    2013-03-01

    An optically transparent thin-layer electrochemical (OTTLE) cell with a locally extended optical path has been developed in order to perform vibrational circular dichroism (VCD) spectroscopy on chiral molecules prepared in specific oxidation states by means of electrochemical reduction or oxidation. The new design of the electrochemical cell successfully addresses the technical challenges involved in achieving sufficient infrared absorption. The VCD-OTTLE cell proves to be a valuable tool for the investigation of chiral redox-active molecules.

  6. Carbon nanotube synthesis via the catalytic chemical vapor deposition of methane in the presence of iron, molybdenum, and iron-molybdenum alloy thin layer catalysts

    Science.gov (United States)

    Yahyazadeh, Arash; Khoshandam, Behnam

    In this study, we documented the catalytic chemical vapor deposition synthesis of carbon nanotubes (CNTs) using ferrocene and molybdenum hexacarbonyl as catalyst nanoparticle precursors and methane as a nontoxic and economical carbon source for the first time. Field emission scanning electron microscopy, energy dispersive X-ray spectroscopy, wavelength dispersive X-ray spectrometry and transmission electron microscopy of the thin layer catalyst as a simple and cost effective catalyst preparation after methane decomposition reaction, along with Fourier transform infrared spectroscopy and Raman spectroscopy confirmed the growth of CNTs, from bimetallic nanoparticles, which are converted into iron-molybdenum alloy nanoparticles at 700 °C for pretreatment by hydrogen after chemical vapor deposition of thin layers. An investigation of the weight percentages of the chemical elements present in the CNTs synthesized from iron-molybdenum catalyst using quartz sheet substrate at 750 °C, confirmed a significant carbon yield of 75.4% which represents high catalyst activity. Additionally, multi-walled carbon nanotubes (∼16-55 nm in diameter and 1.2 μm in length) were observed in the iron-molybdenum alloy sample after methane decomposition reaction at 750 °C for 35 min. To show the role of iron and molybdenum coated on silicon substrate as two thin layer catalysts, samples were considered for CNTs growth (diameter ∼47-69 nm) at 800 °C and 830 °C, respectively. Moreover, the effect of hydrogen pretreatment was evaluated in terms of active metal coating properly. The best graphitic structure due to Raman spectroscopy outcomes (ID/IG ratio) was obtained for iron coated on a quartz sheet, which was estimated at 0.8505. Thermogravimetric analysis proved the thermal stability of the synthesized CNTs using iron thin-layer catalyst up to 350 °C.

  7. Anisotropy adjustment and thickness of thin layer doped by nanoparticules magnetic for the realization of phase matching between fundamental modes in monomode waveguides

    Science.gov (United States)

    Lebbal, M. R.; Boumaza, T.; Bouchemat, M.; Hocini, A.; Hobar, F.; Benghalia, A.; Rosseau, J. J.; Royer, F.

    2008-05-01

    Recently, research has been concentrated on the study of the magnetic nanoparticules for their use in the design of magneto-optical devices. The magneto-optical waveguides for example exploit the Faraday effect to obtain a rotation of polarization TE and TM independent of the propagation direction. In this work, we study isolating component whose operating principle is based on the minimization of the phase mismatch between TE and TM fundamental propagation modes. It appeared promising to use as a guiding film the thin layers doped by magnetic nanoparticules γ-Fe2O3 in order to carry out an adequate phase mismatch. This last can be adjusted by permanent linear birefringence resulting from the application of an external magnetic field during the gelation of the solution which constitutes the guiding film. Many studies were undertaken primarily to minimize the birefringence between TE and TM modes, for that this work represents a new potential means to reach the phase matching by acting on the anisotropy and the thin layer thickness. This condition can be realized in the waveguides with SiO2/TiO2 guiding thin layer doped by nanoparticules of maghemite γ-Fe2O3. The simulations carried out by the FMM method and MATLAB allowed to deduce the conditions to decrease the phase mismatch and increase the conversion ratio of TE/TM modes in order to ameliorate the isolation.

  8. Oxysterols in cosmetics-Determination by planar solid phase extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Schrack, S; Hohl, C; Schwack, W

    2016-11-18

    Sterol oxidation products (SOPs) are linked to several toxicological effects. Therefore, investigation of potential dietary uptake sources particularly food of animal origin has been a key issue for these compounds. For the simultaneous determination of oxysterols from cholesterol, phytosterols, dihydrolanosterol and lanosterol in complex cosmetic matrices, planar solid phase extraction (pSPE) was applied as clean-up tool. SOPs were first separated from more non-polar and polar matrix constituents by normal phase thin-layer chromatography and then focussed into one target zone. Zone extraction was performed with the TLC-MS interface, followed by gas chromatography-mass spectrometry analysis. pSPE showed to be effective for cleaning up cosmetic samples as sample extracts were free of interferences, and gas chromatographic columns did not show any signs of overloading. Recoveries were between 86 and 113% with relative standard deviations of below 10% (n=6). Results of our market survey in 2016 showed that some cosmetics with ingredients of plant origin contained phytosterol oxidation products (POPs) in the low ppm range and therefore in line with levels reported for food. In lanolin containing products, total SOPs levels (cholesterol oxidation products (COPs), lanosterol oxidation products (LOPs), dihydrolanosterol oxidation products (DOPs)) being in the low percent range exceeded reported levels for food by several orders of magnitudes. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. DETERMINATION OF RUTIN IN LEAVES OF SALIX TRIANDRA USING THE METHOD OF PLANAR CHROMATOGRAPHY

    Directory of Open Access Journals (Sweden)

    E. G. Sannikova

    2016-01-01

    Full Text Available The aim of the study is to develop new methods of identification and quantitative determination of rutin in the leaves of Salix triandra L. with thin-layer chromatography. The digital processing of the chromatograms was performed using «Sorbfil Videodensitometer» computer program (Krasnodar. For the chromatography analysis we used plates «Sorbfil» PTSH-P-A-UV, mobile phase: n-butanol-glacial acetic acid-water (4:1:1, detecting reagent – ammonia vapors. The rutin is detected as yellow spots with Rf 0.64±0.02. The detection limit is 0.5 μg/μl. The regression equation has the form: S=4.75×103 m. With the use of this method we found that the composition of rutin in leaves of Salix triandra was in the range 1.81±0.06% on the air-dry raw material (relative standard deviation RSD%=2.5%; the measurement error E=3.12%. The method is sensitive, linear, has a small error, and does not require expensive equipment.

  10. [Regularity of effective carbon numbers of alkanes, alcohols and ethers and its application to determination without authentic standards by gas chromatography].

    Science.gov (United States)

    Sheng, Liyan; Liu, Tingting; Li, Meihua; Pan, Jie; Luo, Yong

    2017-08-08

    To realize quantitative analysis without authentic standards by gas chromatography, a calculation method of effective carbon numbers (ECNs) was developed by determining the relative response factors of 66 alkanes, alcohols, ethers with GC-FID and studying the relation between ECNs and chemical structures. The correlation coefficient of 0.9998 (N=66) was achieved between theoretical values and experimental values of ECNs. Fifty-seven percent of determined compounds had relative deviations within ±1% and all of them had relative deviations within ±3%. This method is as accurate as common internal-standard method while used in the determination of oxygenated chemicals in gasoline samples, but with far less time and economical cost. It could be used to solve the problem of lacking authentic standards or surrogates.

  11. Anti–inflammatory activity and qualitative analysis of different extracts of Maytenus obscura (A. Rich. Cuf. by high performance thin layer chromatography method

    Directory of Open Access Journals (Sweden)

    Mohamed F. Alajmi

    2014-02-01

    Conclusions: HPTLC finger printing of AESF and dichloromethane of Maytenus obscura revealed eight major spots for alcoholic extracts and nine major spots for dichloromethane extracts. These HPTLC profiles may be of great usefulness in the quality control of herbal products containing these extracts. The anti-inflammatory activity of both extracts also revealed the medicinal importance of these extracts. The plant can be further explored for the isolation of phytoconstituents having anti-inflammatory activity.

  12. Construction of a supercritical fluid extraction (SFE) equipment: validation using annatto and fennel and extract analysis by thin layer chromatography coupled to image

    OpenAIRE

    JOHNER,Júlio Cezar Flores; MEIRELES, Maria Angela de Almeida

    2016-01-01

    Abstract The present work describes setting up a laboratory unit for supercritical fluid extraction. In addition to its construction, a survey of cost was done to compare the cost of the homemade unit with that of commercial units. The equipment was validated using an extraction of annatto seeds’ oil, and the extraction and fractionation of fennel oil were used to validate the two separators; for both systems, the solvent was carbon dioxide. The chemical profiles of annatto and fennel e...

  13. Using a Sequence of Experiments with Turmeric Pigments from Food to Teach Extraction, Distillation, and Thin-Layer Chromatography to Introductory Organic Chemistry Students

    Science.gov (United States)

    da S. F. Fagundes, Thayssa; Dutra, Karen Danielle B.; Ribeiro, Carlos Magno R.; de A. Epifanio, Rosa^ngela; Valverde, Alessandra L.

    2016-01-01

    This experiment encourages students to use deductive reasoning skills to understand the correlation between different techniques used in a chemistry laboratory and to extract and analyze curcuminoids using natural products and processed food from a grocery store. Turmeric pigments were used to teach continuous or discontinuous extraction, vacuum…

  14. Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological, pharmaceutical and environmental samples.

    Science.gov (United States)

    Zarzycki, Paweł K; Ślączka, Magdalena M; Zarzycka, Magdalena B; Włodarczyk, Elżbieta; Baran, Michał J

    2011-03-04

    The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds' feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5-8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Low-parachor solvents extraction and thermostated micro-thin-layer chromatography separation for fast screening and classification of spirulina from pharmaceutical formulations and food samples.

    Science.gov (United States)

    Zarzycki, Paweł K; Zarzycka, Magdalena B; Clifton, Vicki L; Adamski, Jerzy; Głód, Bronisław K

    2011-08-19

    The goal of this paper is to demonstrate the separation and detection capability of eco-friendly micro-TLC technique for the classification of spirulina and selected herbs from pharmaceutical and food products. Target compounds were extracted using relatively low-parachor liquids. A number of the spirulina samples which originated from pharmaceutical formulations and food products, were isolated using a simple one step extraction with small volume of methanol, acetone or tetrahydrofuran. Herb samples rich in chlorophyll dyes were analyzed as reference materials. Quantitative data derived from micro-plates under visible light conditions and after iodine staining were explored using chemometrics tools including cluster analysis and principal components analysis. Using this method we could easily distinguish genuine spirulina and non-spirulina samples as well as fresh from expired commercial products and furthermore, we could identify some biodegradation peaks appearing on micro-TLC profiles. This methodology can be applied as a fast screening or fingerprinting tool for the classification of genuine spirulina and herb samples and in particular may be used commercially for the rapid quality control screening of products. Furthermore, this approach allows low-cost fractionation of target substances including cyanobacteria pigments in raw biological or environmental samples for preliminary chemotaxonomic investigations. Due to the low consumption of the mobile phase (usually less than 1 mL per run), this method can be considered as environmentally friendly analytical tool, which may be an alternative for fingerprinting protocols based on HPLC machines and simple separation systems involving planar micro-fluidic or micro-chip devices. Copyright © 2011 Elsevier B.V. All rights reserved.

  16. Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological, pharmaceutical and environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Zarzycki, Pawel K., E-mail: pawel_k_z@hotmail.com [Section of Toxicology and Bioanalytics, Department of Civil and Environmental Engineering, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin (Poland); Slaczka, Magdalena M.; Zarzycka, Magdalena B.; Wlodarczyk, Elzbieta; Baran, Michal J. [Section of Toxicology and Bioanalytics, Department of Civil and Environmental Engineering, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin (Poland)

    2011-03-04

    The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds' feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5-8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.

  17. Reprint of: Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological, pharmaceutical and environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Zarzycki, Pawel K., E-mail: pawel_k_z@hotmail.com [Section of Toxicology and Bioanalytics, Department of Civil and Environmental Engineering, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin (Poland); Slaczka, Magdalena M.; Zarzycka, Magdalena B.; Wlodarczyk, Elzbieta; Baran, Michal J. [Section of Toxicology and Bioanalytics, Department of Civil and Environmental Engineering, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin (Poland)

    2012-02-24

    The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds' feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5-8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.

  18. Micelle Enhanced Fluorimetric and Thin Layer Chromatography Densitometric Methods for the Determination of (± Citalopram and its S – Enantiomer Escitalopram

    Directory of Open Access Journals (Sweden)

    Elham A. Taha

    2009-01-01

    Full Text Available Two sensitive and validated methods were developed for determination of a racemic mixture citalopram and its enantiomer S-(+ escitalopram. The first method was based on direct measurement of the intrinsic fluorescence of escitalopram using sodium dodecyl sulfate as micelle enhancer. This was further applied to determine escitalopram in spiked human plasma, as well as in the presence of common and co-administerated drugs. The second method was TLC densitometric based on various chiral selectors was investigated. The optimum TLC conditions were found to be sensitive and selective for identification and quantitative determination of enantiomeric purity of escitalopram in drug substance and drug products. The method can be useful to investigate adulteration of pure isomer with the cheap racemic form.

  19. High-performance liquid chromatographic enantioseparation of (R,S)-fluoxetine using Marfey's reagent and (S)-N-(4-nitrophenoxycarbonyl) phenylalanine methoxyethyl ester as chiral derivatizing reagents along with direct thin-layer chromatographic resolution and isolation of enantiomers using L-tartaric acid as mobile phase additive.

    Science.gov (United States)

    Bhushan, Ravi; Agarwal, Charu

    2010-11-01

    Chiral assay of enantiomers of fluoxetine was achieved in pharmaceutical formulations using direct and indirect methods. L-tartaric acid was used as a mobile phase additive in thin-layer chromatography; the enantiomers were separated and isolated and were used to determine the elution order in HPLC. (R,S)-flouxetine was derivatized with (S)-N-(4-nitrophenoxycarbonyl)phenylalanine methoxyethyl ester [(S)-NIFE], Marfey's reagent and 1-fluoro-2,4-dinitrophenyl-L-methionine amide (FDNP-L-Met-NH₂. The diastereomers were separated using RP-HPLC. The effect of flow rate and TFA concentration on resolution was studied. The diastereomers obtained by derivatization with FDNP-L-Met-NH₂ were also separated by RP-TLC. Copyright © 2010 John Wiley & Sons, Ltd.

  20. Liquid chromatography-particle beam electron ionization mass spectrometry method for analysis of botanical extracts: evaluation of ephedrine alkaloids in standard reference materials.

    Science.gov (United States)

    Castro, Joaudimir; Krishna, M V Balarama; Marcus, R Kenneth

    2010-01-01

    The preliminary validation of a high-performance liquid chromatography particle beam mass spectrometry method (HPLC-PB/MS) with electron impact ionization source for analysis of botanical extracts is presented. The LC-PB/MS system was evaluated for the analysis of ephedrine alkaloids using ephedra-containing National Institute of Standards and Technology dietary supplement standard reference materials (SRMs) 3241 Ephedra Sinica Stapf Native Extract and 3242 Ephedra Sinica Stapf Commercial Extract. The ephedrine alkaloids were separated by reversed-phase chromatography using a phenyl column at room temperature. A linear gradient method with a mobile phase composition varying from 5:95 [MeOH:0.1% trifluoroacetic acid (TFA) in water] to 20:80 (MeOH:0.1% TFA in water) at a flow rate of 1.0 ml/min, with an analysis time of less than 20 min, was used. The source block temperature was evaluated to determine the optimal operating conditions by monitoring the intensities and fragmentation patterns of the ephedrine alkaloids. Ephedrine and N-methylephedrine were taken as a representative of the test alkaloids. The LODs on the sub-nanogram level were achieved, with ephedrine, pseudoephedrine, and methylephedrine in the SRMs quantified by a standard addition method with recoveries of > or = 86% and RSDs of < or = 14% (n = 3).

  1. Comparison of high-performance liquid chromatographic and thin-layer chromatographic methods for determination of aloin in herbal products containing Aloe vera.

    Science.gov (United States)

    Ramírez Durón, Rosalba; Ceniceros Almaguer, Lucía; Cavazos Rocha, Norma Cecilia; Silva Flores, Perla Giovanna; De Torres, Noemí Waksman

    2008-01-01

    Aloe vera is a medicinal plant used worldwide to treat a variety of conditions and, as such, has important commercial value. Aloin is a principal component of aloe vera leaves and is used for quality control of products containing it. A semiquantitative thin-layer chromatographic (TLC) method for determining the concentration of aloin in aloe-based products was validated. The results were similar to those of a validated high-performance liquid chromatographic method; therefore, TLC, which is a simple, sensitive, specific, rapid, and cheap method, may be ideal for use in any laboratory for routine analysis of commercial products containing aloe vera.

  2. Study of carrier blocking property of poly-linalyl acetate thin layer by electric-field-induced optical second-harmonic generation measurement

    Science.gov (United States)

    Taguchi, Dai; Manaka, Takaaki; Iwamoto, Mitsumasa; Anderson, Liam J.; Jacob, Mohan V.

    2014-02-01

    By using electric-field-induced optical second-harmonic generation (EFISHG) measurement, we studied the carrier-blocking property of poly-linalyl acetate (PLA) thin layers sandwiched in indium-zinc-oxide (IZO)/PLA/C60/Al double-layer diodes. Results showed that the PLA layer totally blocks electrons crossing the C60 layer, and also blocks holes entering from the IZO layer. The EFISHG measurement effectively substantiates the hole-blocking electron-blocking property of the PLA layer sandwiched in double layer diodes.

  3. High-Performance Liquid Chromatographic and High-Performance Thin-Layer Chromatographic Method for Quantitative Estimation of Dolutegravir Sodium in Bulk Drug and Pharmaceutical Dosage Form

    OpenAIRE

    Bhavar, Girija B.; Sanjay S. Pekamwar; Aher, Kiran B.; Thorat, Ravindra S.; Chaudhari, Sanjay R.

    2015-01-01

    Simple, sensitive, precise, and specific high-performance liquid chromategraphic (HPLC) and high-performance thin-layer chromatographic (HPTLC) methods for the determination of dolutegravir sodium in bulk drug and pharmaceutical dosage form were developed and validated. In the HPLC method, analysis of the drug was carried out on the ODS C18 column (150 ? 4.6 mm, 5 ?m particle size) using a mixture of acetonitrile: water (pH 7.5) in the ratio of 80:20 v/v as the mobile phase at the flow rate 1...

  4. Quantitation of formate by solid-phase microextraction and gas chromatography--mass spectrometry utilizing a [13C]formate internal standard.

    Science.gov (United States)

    Kim, Jae Kwang; Shiraishi, Takehiko; Fukusaki, Ei-Ichiro; Kobayashi, Akio

    2003-02-07

    A new method for the analysis of formic acid was developed using gas chromatography-electron impact ionization mass spectrometry in the selected ion monitoring mode and solid-phase microextraction. Using this method with [13C]formic acid as an internal standard, the peak area ratio of [12C]formic acid/[13C]formic acid was not affected by differing methanol or sulfuric acid concentrations during the esterification and fiber adsorbing step. In comparison, the peak area ratio of formic acid/acetonitrile as detected by conventional GC with flame ionization detection was greatly affected by methanol or sulfuric acid concentrations. The formic acid calibration curve of our method showed excellent linearity over the range 5 to 200 microM. The within- and between-run assay relative standard deviations for the formic acid concentration were all less than 1.70%.

  5. Development of standard operating procedure and standardization of Habb-e-Banafsha Qawi-A Unani polyherbal formulation

    Directory of Open Access Journals (Sweden)

    Athar Ali

    2015-01-01

    Full Text Available Introduction: Herbals drugs became a boon for mankind since ancient times and still are used worldwide for the treatment of various human ailments. The safety of alternative medicinal preparations has been questioned due to reports of unwanted side effects. To maintain the quality and efficacy of these drugs, it is essential to standardize them in order to avoid the use of substandard or adulterated medicines in the market. Unani system of medicine mainly focuses on the treatment by natural drugs. Habb-e-Banafsha Qawi is useful in a cough, catarrah, and coryza. Materials and Methods: Physiochemical constants of Habb-e-Banafsha Qawi were determined through organoleptic characters, macro- and micro-scopic characters, ash value, solubility, pH values. Chromatographic fingerprints were developed using thin layer chromatography method. Aflatoxin (AF contamination, heavy metal, and pesticide residues were also evaluated by standard methods.Objectives: In the present study, an attempt has been made to develop standard operating procedure and physiochemical parameters to monitor the quality of a Unani poly-herbal formulation, Habb-e-Banafsha Qawi. Results: The tablets tasted sweetish bitter with a pleasant odor, water soluble and acidic in nature. Rfvalues were almost same in all the extracts. No AF, heavy metal, and pesticide residues were observed. Conclusions: It may be concluded that the values and chromatographic fingerprints obtained can be used for quality evaluation and to set new pharmacopoeial standards for the preparation of Habb-e-Banafsha Qawi.

  6. Rapid resolution liquid chromatography (RRLC) analysis for quality control of Rhodiola rosea roots and commercial standardized products.

    Science.gov (United States)

    Ma, Yuan-Chun; Wang, Xiao-Qiang; Hou, Fei Fei; Ma, Jie; Luo, Mai; Lu, Shane; Jin, Peter; Terevsky, Nelly; Chen, Alice; Xu, Iris; Patel, Asmita V; Gorecki, Dariusz

    2011-05-01

    A simple, sensitive and reliable reversed phase Rapid Resolution Liquid Chromatography (RRLC) method was developed and validated for six biologically active compounds (salidroside, tyrosol, rosarin, rosavin, rosin and rosiridin) in Rhodiola rosea L. roots and powder extracts. The method uses a Phenomenex C18 (2)-HST column at 40 degrees C with a neutral gradient system mobile phase (H20 and acetonitrile), a flow rate of 1.0 mL/min, and UV detection wavelengths set at 205 and 254 nm, simultaneously. Baseline separation of the six active compounds was achieved within 8 minutes. The average percentages of rosavins (rosarin, rosavin, and rosin) in authentic R. rosea roots and root powder extracts were quantitatively determined and a characteristic R. rosea roots RRLC profile was established. The RRLC method is accurate and sensitive; in addition, it effectively increases the sample analysis throughput compared with conventional HPLC.

  7. Investigation of Mach-number effects on roll moment of wrap-around-fin projectiles using thin-layer Navier-Stokes equations

    Energy Technology Data Exchange (ETDEWEB)

    Azimi, A. [Sharif Univ. of Technology, School of Mechanical Engineering, Centre of Excellence in Energy Conversion (CEEC), Tehran (Iran, Islamic Republic of)]. Email: aazimi@mehr.sharif.edu; Fazeli, H. [Sharif Univ. of Technology, School of Mechanical Engineering, Centre of Excellence in Energy Conversion (CEEC), Tehran (Iran, Islamic Republic of)]|[Malek-Ashtar Univ. of Technology, Tehran (Iran, Islamic Republic of); Farhanieh, B. [Sharif Univ. of Technology, School of Mechanical Engineering, Centre of Excellence in Energy Conversion (CEEC), Tehran (Iran, Islamic Republic of)

    2005-07-01

    In this paper, the investigation of Mach-number effects on roll moment of wrap-around-fin projectiles is numerically simulated using a multi-zone approach and the thin-layer Navier-Stokes equations. For computation of the three-dimensional supersonic turbulent flow, averaged thin-layer Navier-Stokes equations in the generalized coordinate system have been solved with an efficient finite-difference factored algorithm of the Beam and Warming. For the turbulent flowfield computations, the well-known isotropic two-layer algebraic eddy viscosity called Baldwin-Lomax model has been used. The case study is a secant-ogive-cylinder configuration with four 34{sup o} swept wrap-around fins at the end of body. To demonstrate the effect of Mach number on aerodynamics coefficients, the aerodynamic characteristics of this configuration including axial force and roll moment for free-stream Mach numbers 1.6-5.0 are presented. In addition, these coefficients are compared with those of the experimental measurements at zero angle of attack and the above Mach numbers, and show good agreement. (author)

  8. Comparative Study on Interface Elements, Thin-Layer Elements, and Contact Analysis Methods in the Analysis of High Concrete-Faced Rockfill Dams

    Directory of Open Access Journals (Sweden)

    Xiao-xiang Qian

    2013-01-01

    Full Text Available This paper presents a study on the numerical performance of three contact simulation methods, namely, the interface element, thin-layer element, and contact analysis methods, through the analysis of the contact behavior between the concrete face slab and the dam body of a high concrete-faced rockfill dam named Tianshengqiao-I in China. To investigate the accuracy and limitations of each method, the simulation results are compared in terms of the dam deformation, contact stress along the interface, stresses in the concrete face slab, and separation of the concrete face slab from the cushion layer. In particular, the predicted dam deformation and slab separation are compared with the in-situ observation data to classify these methods according to their agreement with the in-situ observations. It is revealed that the interface element and thin-layer element methods have their limitations in predicting contact stress, slab separation, and stresses in the concrete face slab if a large slip occurs. The contact analysis method seems to be the best choice whether the separation is finite or not.

  9. Modelling and sequential simulation of multi-tubular metallic membrane and techno-economics of a hydrogen production process employing thin-layer membrane reactor

    KAUST Repository

    Shafiee, Alireza

    2016-09-24

    A theoretical model for multi-tubular palladium-based membrane is proposed in this paper and validated against experimental data for two different sized membrane modules that operate at high temperatures. The model is used in a sequential simulation format to describe and analyse pure hydrogen and hydrogen binary mixture separations, and then extended to simulate an industrial scale membrane unit. This model is used as a sub-routine within an ASPEN Plus model to simulate a membrane reactor in a steam reforming hydrogen production plant. A techno-economic analysis is then conducted using the validated model for a plant producing 300 TPD of hydrogen. The plant utilises a thin (2.5 μm) defect-free and selective layer (Pd75Ag25 alloy) membrane reactor. The economic sensitivity analysis results show usefulness in finding the optimum operating condition that achieves minimum hydrogen production cost at break-even point. A hydrogen production cost of 1.98 $/kg is estimated while the cost of the thin-layer selective membrane is found to constitute 29% of total process capital cost. These results indicate the competiveness of this thin-layer membrane process against conventional methods of hydrogen production. © 2016 Hydrogen Energy Publications LLC

  10. Flexible thin-layer plasma inactivation of bacteria and mold survival in beef jerky packaging and its effects on the meat's physicochemical properties.

    Science.gov (United States)

    Yong, Hae In; Lee, Haelim; Park, Sanghoo; Park, Jooyoung; Choe, Wonho; Jung, Samooel; Jo, Cheorun

    2017-01-01

    The aims of the present study were to examine the use of a flexible thin-layer plasma system in inactivating bacteria and mold on beef jerky in a commercial package and to evaluate the physicochemical changes of the jerky. After plasma treatment for 10min, Escherichia coli O157:H7, Listeria monocytogenes, Salmonella Typhimurium, and Aspergillus flavus populations on the beef jerky were reduced by approximately 2 to 3Log CFU/g. No significant changes in metmyoglobin content, shear force, and myofibrillar fragmentation index were found in the plasma-treated beef jerky. On the other hand, the peroxide content and L ⁎ value were decreased whereas the a ⁎ and ΔE value were increased in the plasma-treated sample. Sensory evaluation indicated negative effects of plasma treatment on flavor, off-odor, and overall acceptability of the beef jerky. In conclusion, the flexible thin-layer plasma system could be employed as a means for decontamination of beef jerky, with slight changes to the physicochemical quality of the product. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. Simultaneous Determination of Four Anthraquinones in Polygoni Multiflori Radix with Single Reference Standard by High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Hua Yang

    2015-07-01

    Full Text Available Objective: To establish a rapid, accurate and reliable analytical method for the simultaneous determination of four major anthraquinones in Polygoni Multiflori Radix (PMR using single reference standard.

  12. An electrostatic precipitator for preparative gas-liquid chromatography.

    Science.gov (United States)

    Borka, L; Privett, O S

    1966-03-01

    The effect of the operating variables of electrostatic precipitators on the recovery and structure of methyl esters and related aerosol forming compounds collected in preparative gas-liquid chromatography was studied.Aerosol formation was prevented by AC or DC voltages of 5000 to 12000 volts. AC was more effective than DC but caused changes in structure which were detectable by both thin-layer and gas-liquid chromatographic methods of analysis.An apparatus of simple construction and operation was designed for the collection of methyl esters and its use demonstrated with several model compounds.

  13. Pharmacognostic and physicochemical standardization of homoeopathic drug: Rumex crispus L.

    Directory of Open Access Journals (Sweden)

    Subramanian Palani

    2016-01-01

    Full Text Available Background: Rumex crispus L., commonly called as "yellow dock" in English, "patience frisee" in French, and "Ampfer" in German, and ′aceda de culebra′ in Spanish is a well-known herb belonging to Polygonaceae. Roots of the herb are used as medicine in homoeopathy. Objective: The pharmacognostic and physicochemical studies on roots have been carried out to enable the use of correct species and standardize the raw material. Materials and Methods: Pharmacognostic studies on roots of authentic raw drug have been carried out; physicochemical parameters, namely, extractive value, ash values, formulation besides weight per mL, total solids, alcohol content along with high-performance thin layer chromatography (HPTLC and ultraviolet studies for mother tincture have been worked out. Results: Roots are blackish-brown, wiry, rounded with irregular striations, tortuous; internally, it is softwood, light-yellow, and fracture fibrous. Phellem is 8-10 layered, discontinuous, and tanniniferous. Phellogen is two-layered and contains inulin crystals in few. Outer phelloderm is 12-16 layered often containing spherocrystals and associated with stone cells. Secondary phloem is up to 25 layered. Xylem is in the form of strips. The physicochemical properties and HPTLC values of the drug are standardized and presented. Conclusion: The powder microscopic features and organoleptic characters along with anatomical and physicochemical studies are diagnostic to establish standards for the drug.

  14. Planar solid phase extraction--a new clean-up concept in multi-residue analysis of pesticides by liquid chromatography-mass spectrometry.

    Science.gov (United States)

    Oellig, Claudia; Schwack, Wolfgang

    2011-09-16

    Efficient clean-up is indispensable for preventing matrix effects in multi-residue analysis of pesticides in food by liquid and gas chromatography coupled to mass spectrometry. As a completely new approach, highly automated planar chromatographic tools were applied for powerful clean-up, called high-throughput planar solid phase extraction (HTpSPE). Thin-layer chromatography (TLC) was used to completely separate pesticides from matrix compounds and to focus them into a sharp zone, followed by extraction of the target zone by the TLC-MS interface. HTpSPE resulted in extracts nearly free of interference and free of matrix effects, as shown for seven chemically representative pesticides in four different matrices (apples, cucumbers, red grapes, tomatoes). Regarding the clean-up step, quantification by LC-MS provided mean recovery (against solvent standards) of 90-104% with relative standard deviations of 0.3-4.1% (n=5) for two spiking levels of 0.1 and 0.5 mg/kg. Clean-up of one sample was completed in a manner of minutes, while running numerous samples in parallel at reduced costs, with very low sample and solvent volumes. Copyright © 2011 Elsevier B.V. All rights reserved.

  15. Atomic Force Microscope Mediated Chromatography

    Science.gov (United States)

    Anderson, Mark S.

    2013-01-01

    The atomic force microscope (AFM) is used to inject a sample, provide shear-driven liquid flow over a functionalized substrate, and detect separated components. This is demonstrated using lipophilic dyes and normal phase chromatography. A significant reduction in both size and separation time scales is achieved with a 25-micron-length column scale, and one-second separation times. The approach has general applications to trace chemical and microfluidic analysis. The AFM is now a common tool for ultra-microscopy and nanotechnology. It has also been demonstrated to provide a number of microfluidic functions necessary for miniaturized chromatography. These include injection of sub-femtoliter samples, fluidic switching, and sheardriven pumping. The AFM probe tip can be used to selectively remove surface layers for subsequent microchemical analysis using infrared and tip-enhanced Raman spectroscopy. With its ability to image individual atoms, the AFM is a remarkably sensitive detector that can be used to detect separated components. These diverse functional components of microfluidic manipulation have been combined in this work to demonstrate AFM mediated chromatography. AFM mediated chromatography uses channel-less, shear-driven pumping. This is demonstrated with a thin, aluminum oxide substrate and a non-polar solvent system to separate a mixture of lipophilic dyes. In conventional chromatographic terms, this is analogous to thin-layer chromatography using normal phase alumina substrate with sheardriven pumping provided by the AFM tip-cantilever mechanism. The AFM detection of separated components is accomplished by exploiting the variation in the localized friction of the separated components. The AFM tip-cantilever provides the mechanism for producing shear-induced flows and rapid pumping. Shear-driven chromatography (SDC) is a relatively new concept that overcomes the speed and miniaturization limitations of conventional liquid chromatography. SDC is based on a

  16. Liquid chromatography-tandem mass spectrometry quantification of 6-thioguanine in DNA using endogenous guanine as internal standard

    DEFF Research Database (Denmark)

    Jacobsen, Jack Hummeland; Schmiegelow, Kjeld; Nersting, Jakob

    2012-01-01

    was estimated at 63% (RSD 26%), which is corrected for by the internal standard resulting in stable quantification. The TG levels found were above the LOQ in 18 out of 18 childhood leukemia patients on 6-mercaptopurine/methotrexate maintenance therapy (median 377, range 45-1190 fmol/μg DNA) with intra...

  17. Internal standards for use in the comprehensive analysis of polychlorinated aromatic hydrocarbons using gas chromatography combined with multiphoton ionization mass spectrometry.

    Science.gov (United States)

    Li, Adan; Imasaka, Totaro

    2016-10-28

    To decrease health-risks to humans, non-toxic compounds were evaluated for use as internal standards for calibrating data obtained by gas chromatography/multiphoton ionization mass spectrometry (GC-MPI-MS) using an ultraviolet femtosecond laser as the ionization source. The retention time in the mass chromatogram was calibrated using a retention index, in which a series of n-alkanes was employed as internal standards for evaluating the retention times for polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), and polychlorinated biphenyls (PCBs). To compensate for changes in signal intensity in MPI-MS, the dependence of signal intensity on the laser pulse energy was investigated for the dioxin-like compounds, in addition to five non-toxic aromatic hydrocarbons, that were used as internal standards. Based on their similar behavior,the non-toxic PCDD/PCDF, its 13C-isotope, and pentachlorobenzene behave similarly, we conclude that they can be used for calibrating the signal intensities in MPI-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Innovative method for carbon dioxide determination in human postmortem cardiac gas samples using headspace-gas chromatography-mass spectrometry and stable labeled isotope as internal standard.

    Science.gov (United States)

    Varlet, V; Smith, F; de Froidmont, S; Dominguez, A; Rinaldi, A; Augsburger, M; Mangin, P; Grabherr, S

    2013-06-19

    A novel approach to measure carbon dioxide (CO2) in gaseous samples, based on a precise and accurate quantification by (13)CO2 internal standard generated in situ is presented. The main goal of this study was to provide an innovative headspace-gas chromatography-mass spectrometry (HS-GC-MS) method applicable in the routine determination of CO2. The main drawback of the GC methods discussed in the literature for CO2 measurement is the lack of a specific internal standard necessary to perform quantification. CO2 measurement is still quantified by external calibration without taking into account analytical problems which can often occur considering gaseous samples. To avoid the manipulation of a stable isotope-labeled gas, we have chosen to generate in situ an internal labeled standard gas ((13)CO2) on the basis of the stoichiometric formation of CO2 by the reaction of hydrochloric acid (HCl) with sodium hydrogen carbonate (NaH(13)CO3). This method allows a precise measurement of CO2 concentration and was validated on various human postmortem gas samples in order to study its efficiency. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. High Pressure Size Exclusion Chromatography (HPSEC) Determination of Dissolved Organic Matter Molecular Weight Revisited: Accounting for Changes in Stationary Phases, Analytical Standards, and Isolation Methods.

    Science.gov (United States)

    McAdams, Brandon C; Aiken, George R; McKnight, Diane M; Arnold, William A; Chin, Yu-Ping

    2018-01-16

    We reassessed the molecular weight of dissolved organic matter (DOM) determined by high pressure size exclusion chromatography (HPSEC) using measurements made with different columns and various generations of polystyrenesulfonate (PSS) molecular weight standards. Molecular weight measurements made with a newer generation HPSEC column and PSS standards from more recent lots are roughly 200 to 400 Da lower than initial measurements made in the early 1990s. These updated numbers match DOM molecular weights measured by colligative methods and fall within a range of values calculated from hydroxyl radical kinetics. These changes suggest improved accuracy of HPSEC molecular weight measurements that we attribute to improved accuracy of PSS standards and changes in the column packing. We also isolated DOM from wetlands in the Prairie Pothole Region (PPR) using XAD-8, a cation exchange resin, and PPL, a styrene-divinylbenzene media, and observed little difference in molecular weight and specific UV absorbance at 280 nm (SUVA 280 ) between the two solid phase extraction resins, suggesting they capture similar DOM moieties. PPR DOM also showed lower SUVA 280 at similar weights compared to DOM isolates from a global range of environments, which we attribute to oxidized sulfur in PPR DOM that would increase molecular weight without affecting SUVA 280 .

  20. Determination of caffeine, theobromine, and theophylline in standard reference material 2384, baking chocolate, using reversed-phase liquid chromatography.

    Science.gov (United States)

    Thomas, Jeanice Brown; Yen, James H; Schantz, Michele M; Porter, Barbara J; Sharpless, Katherine E

    2004-06-02

    A rapid and selective isocratic reversed-phase liquid chromatographic method has been developed at the National Institute of Standards and Technology to simultaneously measure caffeine, theobromine, and theophylline in a food-matrix standard reference material (SRM) 2384, Baking Chocolate. The method uses isocratic elution with a mobile phase composition (volume fractions) of 10% acetronitrile/90% water (pH adjusted to 2.5 using acetic acid) at a flow rate of 1.5 mL/min with ultraviolet absorbance detection (274 nm). Total elution time for these analytes is less than 15 min. Concentration levels of caffeine, theobromine, and theophylline were measured in single 1-g samples taken from each of eight bars of chocolate over an eight-day period. Samples were defatted with hexane, and beta-hydroxyethyltheophylline was added as the internal standard. The repeatability for the caffeine, theobromine, and theophylline measurements was 5.1, 2.3, and 1.9%, respectively. The limit of quantitation for all analytes was theobromine, and theophylline in SRM 2384.

  1. Scanning proximal microscopy study of the thin layers of silicon carbide-aluminum nitride solid solution manufactured by fast sublimation epitaxy

    Directory of Open Access Journals (Sweden)

    Tománek P.

    2013-05-01

    Full Text Available The objective of the study is a growth of SiC/(SiC1−x(AlNx structures by fast sublimation epitaxy of the polycrystalline source of (SiC1−x(AlNx and their characterisation by proximal scanning electron microscopy and atomic force microscopy. For that purpose optimal conditions of sublimation process have been defined. Manufactured structures could be used as substrates for wide-band-gap semiconductor devices on the basis of nitrides, including gallium nitride, aluminum nitride and their alloys, as well as for the production of transistors with high mobility of electrons and also for creation of blue and ultraviolet light emitters (light-emitted diodes and laser diodes. The result of analysis shows that increasing of the growth temperature up to 2300 K allows carry out sublimation epitaxy of thin layers of aluminum nitride and its solid solution.

  2. Pharmacological evaluation and chemical standardization of an ayurvedic formulation for wound healing activity.

    Science.gov (United States)

    Gangopadhyay, Karuna Sagar; Khan, Madhuchanda; Pandit, Srikanta; Chakrabarti, Shrabana; Mondal, Tapan Kumar; Biswas, Tuhin Kanti

    2014-03-01

    Wound healing is a topic of substantial prominence in Ayurveda, the Indian traditional system of medicine. Test drug Kshatantak Malam (KM), otherwise named as Baharer Nani, is described in Ayurveda since a long time for wound healing activity but necessitates scientific base. The test drug was prepared in the form of natural ointment with the plants like Achyranthes aspera, Allium cepa, and Canabis sativa under the base of butter in a specialized form of preparation. Chemical standardization was made on the basis of the physical character, rancidity test, extractive value, thin-layer chromatography, and gas chromatography. An 8-mm-diameter full-thickness punch was produced in Wistar rats. The test drug was applied topically and compared with standard comparators like framycetin ointment and povidone iodine ointment. Effects were observed on the basis of physical parameters like wound contraction size (mm(2)), wound index, healing period (days), tensile strength (g) and biochemical parameters like tissue DNA (mg/g), RNA (mg/g), total protein (mg/g), hydroxyproline (mg/g), PAGE study, and histopathological observations. Significant results (P < .05) were observed with KM in the punch wound model on the basis of various physical, biochemical, and histopathological parameters. The drug was found to be safe in acute and chronic toxicity models in animals. Chemically it is enriched with fatty substances.

  3. Effect of growth on the thermal resistance and survival of Salmonella Tennessee and Oranienburg in peanut butter, measured by a new thin-layer thermal death time device.

    Science.gov (United States)

    Keller, Susanne E; Grasso, Elizabeth M; Halik, Lindsay A; Fleischman, Gregory J; Chirtel, Stuart J; Grove, Stephen F

    2012-06-01

    In published data the thermal destruction of Salmonella species in peanut butter deviates from pseudo-first-order kinetics. The reasons for such deviation are unknown. This study examined both the method used to measure the thermal destruction rate and the method of growth of the microorganisms to explain variations in destruction kinetics. Growth on a solid matrix results in a different physiological state that may provide greater resistance to adverse environments. In this study, Salmonella Tennessee and Oranienburg were grown for 24 h at 37°C under aerobic conditions in broth and agar media to represent planktonic and sessile cell growth, respectively. Peanut butter was held at 25°C and tested for Salmonella levels immediately after inoculation and at various time intervals up to 2 weeks. Thermal resistance was measured at 85°C by use of a newly developed thin-layer metal sample holder. Although thermal heat transfer through the metal device resulted in longer tau values than those obtained with plastic bags (32.5 ± 0.9 versus 12.4 ± 1.9 s), the bags have a relative variability of about 15 % compared with about 3 % in the plates, allowing improved uniformity of sample treatment. The two serovars tested in the thin-layer device showed similar overall thermal resistance levels in peanut butter regardless of growth in sessile or planktonic states. However, thermal destruction curves from sessile cultures exhibited greater linearity than those obtained from planktonic cells (P = 0.0198 and 0.0047 for Salmonella Oranienburg and Salmonella Tennessee, respectively). In addition, both Salmonella serovars showed significantly higher survival in peanut butter at 25°C when originally grown on solid media (P = 0.001) with a survival of Salmonella at different temperatures in a low-water-activity environment such as peanut butter.

  4. Determination of Bitter Orange alkaloids in dietary supplements standard reference materials by liquid chromatography with ultraviolet absorbance and fluorescence detection.

    Science.gov (United States)

    Putzbach, Karsten; Rimmer, Catherine A; Sharpless, Katherine E; Sander, Lane C

    2007-07-13

    Four adrenergic amines [synephrine, octopamine, tyramine, and n-methyltyramine] were determined in a variety of Bitter Orange containing dietary supplements. Two extraction techniques were evaluated in detail: Soxhlet extraction and sonication extraction. A liquid chromatographic separation using a reversed-phase C(18) stationary phase and the ion-pairing reagent sodium dodecyl sulfate was developed to separate the Bitter Orange alkaloids. Ultraviolet absorbance detection at 220 nm and fluorescence detection with excitation at 273 nm and emission at 304 nm were used for the alkaloid detection. The method described was used for the assignment of the levels of the predominant alkaloids in three candidate standard reference materials containing Bitter Orange.

  5. Quantification of target analytes in various biofluids using a postcolumn infused-internal standard method combined with matrix normalization factors in liquid chromatography-electrospray ionization mass spectrometry.

    Science.gov (United States)

    Liao, Hsiao-Wei; Tsai, I-Lin; Chen, Guan-Yuan; Lu, Yen-Shen; Lin, Ching-Hung; Kuo, Ching-Hua

    2014-09-05

    Liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) has become one of the most widely used methods in pharmaceutical laboratories. Although LC-ESI-MS provides high sensitivity and high specificity for quantifying target analytes in complicated biofluids, the associated severe matrix effects (MEs) generally result in large quantification errors. Here, we propose a novel strategy for correcting MEs in various biofluids using a postcolumn infused-internal standard (PCI-IS) method in combination with matrix normalization factors (MNFs). We used the MNFs to normalize the encountered MEs in various biofluids to the MEs encountered in standard solutions. The use of a postcolumn infused-internal standard also corrects the MEs for individual samples. When using the PCI-IS method in combination with MNFs, the calibration curve generated from standard solutions can be applied to quantify the target analytes in various biofluids. We applied this new approach to quantify etoposide and etoposide catechol in plasma and CSF. The accuracy of the test results showed that over 93% of the data have quantification errors less than 20% and that 99% of the data have quantification errors less than 30%. The successful application of this method to evaluate real clinical samples revealed that our proposed MNFs in combination with the PCI-IS method largely simplifies the entire method development and validation processes, saves a great deal of time and cost without sacrificing quantification accuracy, and provides a simple means of quantifying target analytes in various biofluids. This method will be particularly useful in fields in which the same target analytes need to be quantified in various types of matrices, including bioanalysis, forensic toxicology, environmental studies, and food safety control. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Increased Depth and Breadth of Plasma Protein Quantitation via Two-Dimensional Liquid Chromatography/Multiple Reaction Monitoring-Mass Spectrometry with Labeled Peptide Standards.

    Science.gov (United States)

    Percy, Andrew J; Yang, Juncong; Chambers, Andrew G; Borchers, Christoph H

    2016-01-01

    Absolute quantitative strategies are emerging as a powerful and preferable means of deriving concentrations in biological samples for systems biology applications. Method development is driven by the need to establish new-and validate current-protein biomarkers of high-to-low abundance for clinical utility. In this chapter, we describe a methodology involving two-dimensional (2D) reversed-phase liquid chromatography (RPLC), operated under alkaline and acidic pH conditions, combined with multiple reaction monitoring (MRM)-mass spectrometry (MS) (also called selected reaction monitoring (SRM)-MS) and a complex mixture of stable isotope-labeled standard (SIS) peptides, to quantify a broad and diverse panel of 253 proteins in human blood plasma. The quantitation range spans 8 orders of magnitude-from 15 mg/mL (for vitamin D-binding protein) to 450 pg/mL (for protein S100-B)-and includes 31 low-abundance proteins (defined as being proteins for higher sample throughput. Also detailed here is the application of our recently developed software tool-Qualis-SIS-for protein quantitation (via regression analysis of standard curves) and quality assessment of the resulting data. Overall, this chapter provides the blueprint for the replication of this quantitative proteomic method by proteomic scientists of all skill levels.

  7. An artificial aqueous humor as a standard matrix to assess drug concentration in the anterior chamber by high performance liquid chromatography methods.

    Science.gov (United States)

    Macri, Angelo; Marini, Valeria; Sangalli, Giorgio; Fucile, Carmen; Iester, Michele; Mattioli, Francesca

    2015-01-01

    The aim of the study was to recreate in-vitro artificial aqueous humor with the same physico-chemical properties of human aqueous humor to be used as a standard matrix in chromatography to assess drug concentration in the anterior and posterior chamber of the human eye. The artificial aqueous humor was prepared according to the human aqueous humor chemical compositions reported in the literature. The artificial matrix was then analysed via the HPLC-UV method and compared with aqueous humor from 15 patients who underwent cataract surgery. Known concentrations of widely-used ophthalmological drugs were added to the artificial aqueous humor in order to assess whether it can be used to explore ocular disposition towards topically or systemically administered drugs. No significant differences were found between the two examined aqueous humor types. There were no significant qualitative differences between examined fluids in terms of presence of ophthalmological drugs. The composition of artificial, in-vitro recreated aqueous humor was similar to that of the human kind. The absence of significant differences in the analysis of tested drugs both in the artificial and in human aqueous humor indicates that artificial aqueous humor may be used to generate a matrix-based standard curve for analytical method validation.

  8. A New Electrochemical System Based on a Flow-Field Shaped Solid Electrode and 3D-Printed Thin-Layer Flow Cell: Detection of Pb(2+) Ions by Continuous Flow Accumulation Square-Wave Anodic Stripping Voltammetry.

    Science.gov (United States)

    Sun, Qianwen; Wang, Jikui; Tang, Meihua; Huang, Liming; Zhang, Zhiyi; Liu, Chang; Lu, Xiaohua; Hunter, Kenneth W; Chen, Guosong

    2017-05-02

    Here we describe a new and sensitive flow electrochemical detection system that employs a novel flow-field shaped solid electrode (FFSSE). The system was constructed with a 3D-printed thin-layer flow cell (TLFC) and a flat screen-printed FFSSE with USB connection. This interface facilitates continuous flow accumulation square-wave anodic stripping voltammetry (ASV). The flow distribution in the working space of TLFC was simulated using the finite element method (FEM) and the shape and configuration of electrodes were optimized accordingly. We demonstrated the electrochemical determination of Pb(2+) using this newly designed TLFC-FFSSE detection system without removal of oxygen from samples. This TLFC-FFSSE based system showed an attractive stripping voltammetric performance compared to a traditional ASV based method. A linear range for detection of Pb(2+) was found to be 0.5-100 μg/L (0.5 to 100 ppb) and a detection limit of 0.2 μg/L (0.2 ppb) was achieved in the presence of bismuth as codeposition metal. The system was further applied to detect Pb(2+) in biological broths of methane fermentation. The electrochemical detection results were consistent with that obtained from atomic fluorescence spectroscopy (AFS) analysis and the average recovery was found to be 95.5-106.5% using a standard addition method. This new flow electrochemical detection system showed better sensitivity and reproducibility compared to a traditional ASV based method. Such a system offers great potential for on-site and real-time detection of heavy metals where compact, inexpensive, robust, and low-volume analysis is required.

  9. Stable Chlorine Isotopes and Elemental Chlorine by Thermal Ionization Mass Spectrometry and Ion Chromatography; Martian Meteorites, Carbonaceous Chondrites and Standard Rocks

    Science.gov (United States)

    Nakamura, N.; Nyquist, L. E.; Reese, Y.; Shih, C.-Y.; Fujitani, T.; Okano, O.

    2011-01-01

    Recently significantly large mass fractionation of stable chlorine isotopes has been reported for terrestrial and lunar samples [1,2]. In addition, in view of possible early solar system processes [3] and also potential perchlorate-related fluid/microbial activities on the Martian surface [4,5], a large chlorine isotopic fractionation might be expected for some types of planetary materials. Due to analytical difficulties of isotopic and elemental analyses, however, current chlorine analyses for planetary materials are controversial among different laboratories, particularly between IRMS (gas source mass spectrometry) and TIMS (Thermal Ionization Mass Spectrometry) groups [i.e. 1,6,7] for isotopic analyses, as well as between those doing pyrohydrolysis and other groups [i.e. 6,8]. Additional careful investigations of Cl isotope and elemental abundances are required to confirm real chlorine isotope and elemental variations for planetary materials. We have developed a TIMS technique combined with HF-leaching/ion chromatography at NASA JSC that is applicable to analysis of small amounts of meteoritic and planetary materials. We present here results for several standard rocks and meteorites, including Martian meteorites.

  10. One single standard substance for the simultaneous determination of 17 triterpenes in Ganoderma lingzhi and its related species using high-performance liquid chromatography.

    Science.gov (United States)

    Liu, Wei; Zhang, Jingsong; Han, Wei; Liu, Yanfang; Feng, Jie; Tang, Chuanhong; Feng, Na; Tang, Qingjiu

    2017-11-15

    Due to the difficulty and high cost for the preparation of triterpenes, one single standard for the simultaneous determination of multi-components (SSDMC) with high performance liquid chromatography (HPLC) is an advanced solution for multi-component analysis. Experiments were carried out to investigate the feasibility of SSDMC for the analysis of Ganoderma triterpenes, with external standard method (ESM) compared, and the samples of Ganoderma were classified by the content of Ganoderma triterpenes. The analysis was performed by using a Fortis Speed Core-C18 column (150mm×4.6mm I.D., 2.6μm) at gradient elution of 0.01% glacial acetic acid-water (V/V) and acetonitrile with diode array detection (252nm), at a flow rate of 1mL/min. The results showed that all calibration curves had good linearity (r 2 >0.9999) within test ranges. The LOD and LOQ were lower than 2.52ng and 6.43ng, respectively. The RSD for intra-day and inter-day of the seventeen analytes were less than 3.12% at three levels, and the recoveries were 91.4-103.0%. The contents of other 16 triterpenes were determined with ganoderic acid A by SSDMC, which showed that there were few differences compared with the results obtained by ESM. Moreover, the classification of 25 different species and strains of Ganoderma by using the content of triterpenes intuitively reflected the distinction among Ganoderma. In summary, the developed method could be readily utilized as a method of quality evaluation for Ganoderma triterpenes. Copyright © 2017. Published by Elsevier B.V.

  11. Standardization and in vitro antioxidant activity of jatamansi rhizome

    Directory of Open Access Journals (Sweden)

    Mhaveer Singh

    2015-01-01

    Full Text Available Background: Nardostachys jatamansi Linn. commonly known as jatamansi is a well notorious drug in Indian systems of medicines having various health-related benefits and employed in various herbal formulations due to the presence of high levels of valuable phenolic constituents. The present study was aimed to quality assessment of Jatamansi rhizome by studying macro- and micro-scopic characters along with physicochemical tests, chemo-profiling using thin layer chromatography (TLC, and gas chromatography–mass spectrometry (GC-MS, in vitro antioxidant activity. Materials and Methods: Standardization was carried out as per the pharmacopeial guidelines and contaminant estimation was carried out by analyzing the samples for the determination of heavy metals, pesticides, and aflatoxins. Chemo-profiling was done with TLC by optimizing the mobile phase for different extracts. The GC-MS chemo-profiling was also carried out by using hexane soluble fraction of the hydroalcoholic extract. The drug is well known for a protective role in the human body as an antioxidant, so total phenolic contents and in vitro antioxidant efficacy was also determined by using established methods. Results:The results of quality control and anatomical studies were very much useful for its identification, whereas significant antioxidant efficacy was also observed. The drug was found free of contaminants when analyzed for pesticides and aflatoxins, whereas heavy metals were found under the pharmacopeial limit. Conclusion: The findings of the present research can be utilized for the identification and quality control of the jatamansi rhizome.

  12. Optical-to-optical interface device. [consisting of two transparent electrodes on glass substrates that enclose thin film photoconductor and thin layer of nematic liquid crystal

    Science.gov (United States)

    Jacobson, A. D.

    1973-01-01

    Studies were conducted on the performance of a photoactivated dc liquid crystal light valve. The dc light valve is a thin film device that consists of two transparent electrodes, deposited on glass substrates, that enclose a thin film photoconductor (cadmium sulfide) and a thin layer of a nematic liquid crystal that operates in the dynamic scattering mode. The work was directed toward application of the light valve to high resolution non-coherent light to coherent light image conversion. The goal of these studies was to improve the performance and quality of the already existing dc light valve device and to evaluate quantitatively the properties and performance of the device as they relate to the coherent optical data processing application. As a result of these efforts, device sensitivity was improved by a factor of ten, device resolution was improved by a factor of three, device lifetime was improved by two-orders of magnitude, undesirable secondary liquid crystal scattering effects were eliminated, the scattering characteristics of the liquid crystal were thoroughly documented, the cosmetic quality of the devices was dramatically improved, and the performance of the device was fully documented.

  13. The thin layer technique and its application to electron microscopy; La technique des couches minces et son application a la microscopie electronique

    Energy Technology Data Exchange (ETDEWEB)

    Ranc, G. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1957-10-15

    This work deals with the technique of thin layers obtained by evaporation under vacuum, in the thickness range extending from a few monoatomic layers to several hundred angstroms. The great theoretical and practical interest of these layers has, it is well known, given rise to many investigations from Faraday onwards. Within the necessarily restricted limits of this study, we shall approach the problem more particularly from the point of view of: - their production; - their use in electron microscopy. A critical appraisal is made, in the light of present-day knowledge, based on our personal experience and on an extensive bibliography which we have collected on the subject. (author) [French] Le present travail concerne la technique des couches minces obtenues par evaporation sous vide, dans le domaine d'epaisseur qui s'etend de quelques couches monoatomiques a plusieurs centaines d'angstroms. L'interet theorique et pratique considerable de ces couches a suscite, comme on sait, de nombreux travaux depuis Faraday. Dans le cadre necessairement restreint de cette these, nous aborderons plus particulierement le point de vue de: - leur obtention; - leur utilisation en microscopie electronique. Il s'agit d'une mise au point critique, a la lumiere des connaissances actuelles, appuyee sur notre experience personnelle et sur une importante bibliographie, qu'il nous a ete donne de reunir a ce sujet. (auteur)

  14. Development and validation of a simple thin-layer chromatographic method for the analysis of p-chlorophenol in treated wastewater

    Directory of Open Access Journals (Sweden)

    Tešić Živoslav

    2012-01-01

    Full Text Available A thin-layer chromatographic method with densitometric detection was established for quantification of p-chlorophenol in waste water. Degradation efficiency of p-chlorophenol was monitored after each treatment of the wastewater samples. Degradation of p-chlorophenol was performed with advanced oxidation processes (AOPs, using UV, H2O2/UV, O3/H2O2/UV, O3 and O3/UV. Developed TLC procedure has been found to be simple, rapid and precise. The method was characterized by high sensitivity (limit of detection was 11 ng per band and limit of quantification 35 ng per band, linear range (from 75 to 500 ng per band, r = 0.9965, and high precision, accuracy (mean percentage recovery 98.6%, and specificity. Additionally, the efficiency of degradation was monitored using HPLC giving comparable results with RP TLC measurements. [Acknowledgement. This work was performed within the framework of the research project No. 172017 supported by the Ministry of Education and Science of Serbia.

  15. Effect of deflocculation on photo induced thin layer titanium dioxide disintegration of dairy waste activated sludge for cost and energy efficient methane production.

    Science.gov (United States)

    Sharmila, V Godvin; Dhanalakshmi, P; Rajesh Banu, J; Kavitha, S; Gunasekaran, M

    2017-11-01

    In the present study, the deflocculated sludge was disintegrated through thin layer immobilized titanium dioxide (TiO2) as photocatalyst under solar irradiation. The deflocculation of sludge was carried out by 0.05g/g SS of sodium citrate aiming to facilitate more surface area for subsequent TiO2 mediated disintegration. The proposed mode of disintegration was investigated by varying TiO2 dosage, pH and time. The maximum COD solubilization of 18.4% was obtained in the optimum 0.4g/L of TiO2 dosage with 5.5 pH and exposure time of 40min. Anaerobic assay of disintegrated samples confirms the role of deflocculation as methane yield was found to be higher in deflocculated (235.6mL/gVS) than the flocculated sludge (146.8mL/gVS). Moreover, the proposed method (Net cost for control - Net cost for deflocculation) saves sludge management cost of about $132 with 53.8% of suspended solids (SS) reduction. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. High-performance thin-layer chromatography analysis of steviol glycosides in Stevia formulations and sugar-free food products, and benchmarking with (ultra) high-performance liquid chromatography.

    Science.gov (United States)

    Morlock, Gertrud E; Meyer, Stephanie; Zimmermann, Benno F; Roussel, Jean-Marc

    2014-07-11

    A high-performance TLC (HPTLC) method was newly developed and validated for analysis of 7 steviol glycosides in 6 different types of food and Stevia formulations. After a minimized one-step sample preparation, 21 samples were developed in parallel, allowing an effective food screening. Depending on the sample application volume, the method was suited to analyze food sample concentrations in the mg/kg range. LOQs of stevioside in natural yoghurt matrix spiked at 0.02, 0.13 and 0.2% were determined by the calibration curve method to be 12ng/band (peak height). ANOVA was successfully passed to prove data homogeneity in the working range (30-600ng/band). The accuracy (recovery tolerance limit, 92-120%), repeatability (3.1-5.4%) and intermediate precision (4.0-8.4%) were determined for stevioside in milk-based matrix including sample preparation and recovery rates at 3 different concentration levels. For the first time, the recording of HPTLC-ESI-MS spectra via the TLC-MS Interface was demonstrated for rebaudioside A. HPTLC contents for rebaudioside A were compared with results of two (U)HPLC methods. The running costs and analysis time of the three different methods were discussed in detail with regard to screening of food products. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Identification of Ginkgo biloba supplements adulteration using high performance thin layer chromatography and ultra high performance liquid chromatography-diode array detector-quadrupole time of flight-mass spectometry

    Science.gov (United States)

    Ginkgo biloba is one of the most widely sold herbal supplements and medicines in the world. Its popularity stems to have a positive effect on memory and the circulatory system in clinical studies. As ginkgo popularity increased, non-proprietary extracts were introduced claiming to have similar phyto...

  18. Development of a high-performance liquid chromatography method for the determination of florfenicol in animal feedstuffs.

    Science.gov (United States)

    Yang, JinJing; Sun, GuiZhi; Qian, MingRong; Huang, LingLi; Ke, XianBing; Yang, Bo

    2017-11-15

    An effective thin layer chromatography (TLC) purification procedure coupled to high-performance liquid chromatography (HPLC) method was developed for the determination of florfenicol (FF) in pig, chicken and fish feedstuffs. The feedstuff samples were extracted with ethyl acetate, defatted with n-hexane saturated with acetonitrile, and further purified by TLC. The chromatographic separation was performed on a Waters Symmetry C18 column using an isocratic procedure with acetonitrile-water (35:65, v/v) at 0.6mL/min. The ultraviolet (UV) detector was set at a wavelength of 225nm. The FF concentrations in feedstuff samples were quantified using a standard curve. Good linear correlations (y=159075x-15054, r>0.9999) were achieved within the concentration range of 0.05-200μg/mL. The recoveries of FF spiked at levels of 1, 100 and 1000μg/g ranged from 80.6% to 105.3% with the intra-day and inter-day relative standard deviation (RSD) less than 9.3%. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.02 and 0.06mg/kg for pig feedstuffs, 0.02 and 0.07mg/kg for chicken feedstuffs, and 0.02 and 0.05mg/kg for fish feedstuffs, respectively. This reliable, simple and cost-effective method could be applied to the routine monitoring of FF in animal feedstuffs. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Evaluation of cannabinoids concentration and stability in standardized preparations of cannabis tea and cannabis oil by ultra-high performance liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Pacifici, Roberta; Marchei, Emilia; Salvatore, Francesco; Guandalini, Luca; Busardò, Francesco Paolo; Pichini, Simona

    2017-08-28

    Cannabis has been used since ancient times to relieve neuropathic pain, to lower intraocular pressure, to increase appetite and finally to decrease nausea and vomiting. The combination of the psychoactive cannabis alkaloid Δ9-tetrahydrocannabinol (THC) with the non-psychotropic alkaloids cannabidiol (CBD) and cannabinol (CBN) demonstrated a higher activity than THC alone. The Italian National Institute of Health sought to establish conditions and indications on how to correctly use nationally produced cannabis to guarantee therapeutic continuity in individuals treated with medical cannabis. The evaluation of cannabinoids concentration and stability in standardized preparations of cannabis tea and cannabis oil was conducted using an easy and fast ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) assay. Extraction efficiency of oil was significantly higher than that of water with respect to the different cannabinoids. This was especially observed in the case of the pharmacologically active THC, CBD and their acidic precursors. Fifteen minutes boiling was sufficient to achieve the highest concentrations of cannabinoids in the cannabis tea solutions. At ambient temperature, a significant THC and CBD decrease to 50% or less of the initial concentration was observed over 3 and 7 days, respectively. When refrigerated at 4 °C, similar decreasing profiles were observed for the two compounds. The cannabinoids profile in cannabis oil obtained after pre-heating the flowering tops at 145 °C for 30 min in a static oven resulted in a complete decarboxylation of cannabinoid acids CBDA and THCA-A. Nevertheless, it was apparent that heat not only decarboxylated acidic compounds, but also significantly increased the final concentrations of cannabinoids in oil. The stability of cannabinoids in oil samples was higher than that in tea samples since the maximum decrease (72% of initial concentration) was observed in THC coming from unheated flowering

  20. Preparation of bone-implants by coating hydroxyapatite nanoparticles on self-formed titanium dioxide thin-layers on titanium metal surfaces.

    Science.gov (United States)

    Wijesinghe, W P S L; Mantilaka, M M M G P G; Chathuranga Senarathna, K G; Herath, H M T U; Premachandra, T N; Ranasinghe, C S K; Rajapakse, R P V J; Rajapakse, R M G; Edirisinghe, Mohan; Mahalingam, S; Bandara, I M C C D; Singh, Sanjleena

    2016-06-01

    Preparation of hydroxyapatite coated custom-made metallic bone-implants is very important for the replacement of injured bones of the body. Furthermore, these bone-implants are more stable under the corrosive environment of the body and biocompatible than bone-implants made up of pure metals and metal alloys. Herein, we describe a novel, simple and low-cost technique to prepare biocompatible hydroxyapatite coated titanium metal (TiM) implants through growth of self-formed TiO2 thin-layer (SFTL) on TiM via a heat treatment process. SFTL acts as a surface binder of HA nanoparticles in order to produce HA coated implants. Colloidal HA nanorods prepared by a novel surfactant-assisted synthesis method, have been coated on SFTL via atomized spray pyrolysis (ASP) technique. The corrosion behavior of the bare and surface-modified TiM (SMTiM) in a simulated body fluid (SBF) medium is also studied. The highest corrosion rate is found to be for the bare TiM plate, but the corrosion rate has been reduced with the heat-treatment of TiM due to the formation of SFTL. The lowest corrosion rate is recorded for the implant prepared by heat treatment of TiM at 700 °C. The HA-coating further assists in the passivation of the TiM in the SBF medium. Both SMTiM and HA coated SMTiM are noncytotoxic against osteoblast-like (HOS) cells and are in high-bioactivity. The overall production process of bone-implant described in this paper is in high economic value. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Influence of drying conditions on the effective moisture diffusivity, energy of activation and energy consumption during the thin-layer drying of berberis fruit (Berberidaceae)

    Energy Technology Data Exchange (ETDEWEB)

    Aghbashlo, Mortaza; Kianmehr, Mohammad H.; Samimi-Akhijahani, Hadi [Department of Agriculture Machinery, University of Tehran, Aboreyhan Campus (Iran)

    2008-10-15

    Berberis is known as a medicinal and ornamental plant in the world. Berberis fruit is used in medicine to cure liver, neck and stomach cancer, blood purification and mouth scent. Dried berberis fruit using new technology was preserved for relatively long time. Thin-layer drying simulation was used to obtain experiment data, using laboratory scale hot-air dryer of the static tray. Fick's second law was used as a major equation to calculate the moisture diffusivity with some simplification. The calculated value of moisture diffusivity varied from a minimum of 3.320 x 10{sup -10} to a maximum of 9 x 10{sup -9} m{sup 2}/s and the value of energy activation from a minimum of 110.837 to a maximum of 130.61 kJ/mol of from 50 C to 70 C with drying air velocities of 0.5-2 m/s. The high value of the energy of activation for berberis fruit probably related to the tissue of berberis fruit and high moisture content (about 74.28%w.b), and intensive changes in D{sub eff} values for a different air temperature at constant air velocity. The input energy values and specific energy requirement for thin-drying of berberis fruit were found to be in the range of 0.643348-35.20032 (kWh) and 20.9355-1110.0700 (kWh/kg) from 50 C to 70 C with drying air velocities of 0.5-2 m/s, respectively. (author)

  2. Validated stability-indicating high performance thin layer chromatographic method for determination of Ivabradine hydrochloride in bulk and marketed formulation: An application to kinetic study

    Directory of Open Access Journals (Sweden)

    Mitesh H. Motisariya

    2013-12-01

    Full Text Available A sensitive, selective, precise and accurate stability-indicating high-performance thin layer chromatographic method for analysis of Ivabradine hydrochloride (IH an anti anginal agent, both as a bulk drug and in formulations was developed and validated according to ICH guideline. Densitometric analysis of IH was carried out in the absorbance mode at 287 nm using ethyl acetate: 0.389 M ammonium acetate in methanol (1:5, v/v as solvent system. This system was found to give compact spots for IH at an Rf value of 0.36 ± 0.01. Moreover, IH was subjected to acid and alkali hydrolysis, oxidation, accelerated humidity/temperature, wet heat treatment, and photo degradation. The drug undergoes degradation under mainly acidic and basic conditions. Also the degraded products were well resolved from the pure drug with significantly different Rf values. Linearity was found to be in the range of 1200–2800 ng/band. The LOD and LOQ for IH were 255.86 ng/band and 775.33 ng/band, respectively. “Bartlett’s test” and “Lack of fit” applied on peak area for linearity, additionally proved validity of the developed method. Good accuracy and precision were obtained as revealed from %RSD value less than 2. Similarly, no interference was observed from common excipients in tablet formulation as well as degradation product, indicating specificity of the method. As the method could effectively separate the drug from its degradation product, it can be employed as a stability-indicating one. Moreover, proposed method was also utilized to investigate the kinetics of acidic degradation process at different temperatures and first order rate constant, half-life, shelf-life and activation energy were calculated.

  3. A Lithium Ion Highway by Surface Coordination Polymerization: In Situ Growth of Metal-Organic Framework Thin Layers on Metal Oxides for Exceptional Rate and Cycling Performance.

    Science.gov (United States)

    Han, Yuzhen; Yu, Danni; Zhou, Junwen; Xu, Peiyu; Qi, Pengfei; Wang, Qianyou; Li, Siwu; Fu, Xiaotao; Gao, Xing; Jiang, Chenghao; Feng, Xiao; Wang, Bo

    2017-08-25

    A thin layer of a highly porous metal-organic framework material, ZIF-8, is fabricated uniformly on the surface of nanostructured transition metal oxides (ZnO nanoflakes and MnO2 nanorods) to boost the transfer of lithium ions. The novel design and uniform microstructure of the MOF-coated TMOs (ZIF-8@TMOs) exhibit dramatically enhanced rate and cycling performance comparing to their pristine counterparts. The capacities of ZIF-8@ZnO (nanoflakes) and ZIF-8@MnO2 (nanorods) are 28 % and 31 % higher that of the pristine ones at the same current density. The nanorods of ZIF-8@MnO2 show a capacity of 1067 mAh g-1 after 500 cycles at 1 Ag-1 and without any fading. To further improve the conductivity and capacity, the ZIF-8-coated materials are pyrolyzed at 700 °C in an N2 atmosphere (ZIF-8@TMO-700 N). After pyrolysis, a much higher capacity improvement is achieved: ZIF-8@ZnO-700 N and ZIF-8@MnO2 -700 N have 54 % and 69 % capacity increases compared with the pristine TMOs, and at 1 Ag-1 , the capacity of ZIF-8@MnO2 -700 N is 1060 mAh g-1 after cycling for 300 cycles. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. High-Performance Liquid Chromatographic and High-Performance Thin-Layer Chromatographic Method for the Quantitative Estimation of Dolutegravir Sodium in Bulk Drug and Pharmaceutical Dosage Form.

    Science.gov (United States)

    Bhavar, Girija B; Pekamwar, Sanjay S; Aher, Kiran B; Thorat, Ravindra S; Chaudhari, Sanjay R

    2016-01-01

    Simple, sensitive, precise, and specific high-performance liquid chromategraphic (HPLC) and high-performance thin-layer chromatographic (HPTLC) methods for the determination of dolutegravir sodium in bulk drug and pharmaceutical dosage form were developed and validated. In the HPLC method, analysis of the drug was carried out on the ODS C18 column (150 × 4.6 mm, 5 μm particle size) using a mixture of acetonitrile: water (pH 7.5) in the ratio of 80:20 v/v as the mobile phase at the flow rate 1 mL/min at 260 nm. This method was found to be linear in the concentration range of 5-35 μg/mL. The peak for dolutegravir sodium was observed at 3.0 ± 0.1 minutes. In the HPTLC method, analysis was performed on aluminum-backed plates pre-coated with silica gel G60 F254 using methanol: chloroform: formic acid in the proportion of 8:2:0.5 v/v/v as the mobile phase. This solvent system was found to give compact spots for dolutegravir sodium with the Rf value 0.77 ± 0.01. Densitometric analysis of dolutegravir sodium was carried out in the absorbance mode at 265 nm. Linear regression analysis showed good linearity with respect to peak area in the concentration range of 200-900 ng/spot. The methods were validated for precision, limit of detection (LOD), limit of quantitation (LOQ), accuracy, and specificity. Statistical analysis showed that both of the methods are repeatable and specific for the estimation of the said drug. The methods can be used for routine quality control analysis of dolutegravir sodium.

  5. Effects of bath composition on the morphology of electroless-plated Cu electrodes for hetero-junctions with intrinsic thin layer solar cell

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Woon Young [Surface Technology R& BD Group, Korea Institute of Industrial Technology (KITECH), Gaetbeol-ro 156, Yeonsu-gu, Incheon 406-840 (Korea, Republic of); Lee, Yu Jin [Surface Technology R& BD Group, Korea Institute of Industrial Technology (KITECH), Gaetbeol-ro 156, Yeonsu-gu, Incheon 406-840 (Korea, Republic of); Department of Materials Science & Engineering, Yonsei University, Yonsei-ro 50, Seodaemun-Gu, Seoul 120-749 (Korea, Republic of); Lee, Min Hyung, E-mail: minhyung@kitech.re.kr [Surface Technology R& BD Group, Korea Institute of Industrial Technology (KITECH), Gaetbeol-ro 156, Yeonsu-gu, Incheon 406-840 (Korea, Republic of)

    2015-07-31

    The morphology of an electroless-plated Cu electrode was investigated as a function of bath composition. To enhance the selectivity of Cu electrode deposition on the surface of an indium tin oxide layer, a Ti/Cu multi-layer was deposited as a Cu electrode seed layer by physical vapor deposition, and then electroless plating was performed using various complexing agents and a surfactant. The degree of selectivity was effectively influenced by the type of complexing agent. The electroless plating solution containing N,N,N′,N′-tetrakis(2-hydroxypropyl)ethylenediamine (THPED) as complexing agent showed excellent selective growth of the Cu electrode as compared to the solution containing ethylenediaminetetraacetic acid. Even though THPED led to better selective growth of the electroless-plated Cu electrode, the aspect ratio of electrode lateral growth was about 2.7 times that of vertical growth. By adding a nonionic surfactant, the ratio between vertical growth rate and lateral growth rate was improved about 4.6 times. The Cu–THPED electroless plating with nonionic surfactant provided a drastic decrease in lateral growth rate, compared with the Cu–THPED electroless plating bath excluding nonionic surfactant. The Cu–THPED solution including nonionic surfactant is a promising composition of electroless plating solution for the clear selective plating of Cu electrodes on hetero-junctions with intrinsic thin layer solar cells. - Highlights: • Selective electroless plating (SEP) depends on binding strength of complexing agent. • The SEP was performed using Cu-N,N,N′,N′-tetrakis(2-hydroxypropyl)ethylenediamine. • A surfactant is able to remove hydrogen bubbles on Cu electrode surface. • The growth of Cu electrode was improved in vertical direction by adding surfactant.

  6. Preparation of bone-implants by coating hydroxyapatite nanoparticles on self-formed titanium dioxide thin-layers on titanium metal surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Wijesinghe, W.P.S.L.; Mantilaka, M.M.M.G.P.G.; Chathuranga Senarathna, K.G. [Department of Chemistry, Faculty of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Herath, H.M.T.U. [Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Department of Medical Laboratory Science, Faculty of Allied Health Sciences, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Premachandra, T.N. [Department of Veterinary Pathobiology, Faculty of Veterinary Medicine, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Ranasinghe, C.S.K. [Department of Chemistry, Faculty of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Rajapakse, R.P.V.J. [Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Department of Veterinary Pathobiology, Faculty of Veterinary Medicine, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Rajapakse, R.M.G., E-mail: rmgr@pdn.ac.lk [Department of Chemistry, Faculty of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Postgraduate Institute of Science, University of Peradeniya, 20400 Peradeniya (Sri Lanka); Edirisinghe, Mohan; Mahalingam, S. [Department of Mechanical Engineering, University College London, London WC1E 7JE (United Kingdom); Bandara, I.M.C.C.D. [School of Chemistry, Physics and Mechanical Engineering, Queensland University of Technology, 2 George Street, Brisbane 4001, QLD (Australia); Singh, Sanjleena [Central Analytical Research Facility, Institute of Future Environments, Queensland University of Technology, 2 George Street, Brisbane 4001, QLD (Australia)

    2016-06-01

    Preparation of hydroxyapatite coated custom-made metallic bone-implants is very important for the replacement of injured bones of the body. Furthermore, these bone-implants are more stable under the corrosive environment of the body and biocompatible than bone-implants made up of pure metals and metal alloys. Herein, we describe a novel, simple and low-cost technique to prepare biocompatible hydroxyapatite coated titanium metal (TiM) implants through growth of self-formed TiO{sub 2} thin-layer (SFTL) on TiM via a heat treatment process. SFTL acts as a surface binder of HA nanoparticles in order to produce HA coated implants. Colloidal HA nanorods prepared by a novel surfactant-assisted synthesis method, have been coated on SFTL via atomized spray pyrolysis (ASP) technique. The corrosion behavior of the bare and surface-modified TiM (SMTiM) in a simulated body fluid (SBF) medium is also studied. The highest corrosion rate is found to be for the bare TiM plate, but the corrosion rate has been reduced with the heat-treatment of TiM due to the formation of SFTL. The lowest corrosion rate is recorded for the implant prepared by heat treatment of TiM at 700 °C. The HA-coating further assists in the passivation of the TiM in the SBF medium. Both SMTiM and HA coated SMTiM are noncytotoxic against osteoblast-like (HOS) cells and are in high-bioactivity. The overall production process of bone-implant described in this paper is in high economic value. - Highlights: • Colloidal hydroxyapatite nanorods are prepared by a novel method. • Surfaces of titanium metal plates are modified by self-forming TiO{sub 2} thin-films. • Prostheses are prepared by coating hydroxyapatite on surface modified Ti metal. • Bioactivity and noncytotoxicity are increased with surface modifications.

  7. Pharmacognostic standardization of Homoeopathic drug: Juniperus virginiana L.

    Directory of Open Access Journals (Sweden)

    P Padma Rao

    2015-01-01

    Full Text Available Background: Juniperus virginiana L., commonly known as ′red cedar′ in English is a well-known evergreen tree belonging to the family Cupressaceae. The leaves and young aerial shoots are used for preparation of medicine in Homoeopathy. Objective: Standardization is the quintessential aspect which ensures purity and quality of drugs. Hence, the pharmacognostic and physico-chemical studies are carried out to facilitate the use of authentic and correct species of raw drug plant material with established parametric standards for manufacturing the drug. Materials and Methods: Pharmacognostic studies on leaves and young aerial parts of authentic samples of J. virginiana L. have been carried out; physico-chemical parameters of raw drug viz., extractive values, ash values, formulation, besides weight per mL, total solids, alcohol content along with High Performance Thin Layer Chromatography (HPTLC and ultraviolet visible studies have been worked out for mother tincture. Results: The leaves are needles, narrow and sharp at tips; stems are round with greyish white to brown bark possessing small lenticels and covered by imbricate leaves. Epidermal cells in the surface have polygonal linear sides with pitted walls containing crystals and starch. Stomata exclusively occur on the adaxial surface in linear rows. Hypodermis of leaf in T.S. is marked with 1-2 layered lignified sclerenchyma. 2-4 secretory canals are present with one conspicuously beneath midvein bundle. The young terminal axis is sheathed by two closely surrounding leaves while the mature stem possess four leaf bases attached. Vascular tissue of stem possesses predominant xylem surrounded by phloem containing sphaeraphides, prismatic crystals and starch grains. Uniseriate rays occur in the xylem. Mature stem possess shrivelled cork, followed by the cortex. Physicochemical properties and HPTLC values of the drug are standardized and presented. Conclusion: The powder microscopic features and

  8. Layer chromatography-bioassays directed screening and identification of antibacterial compounds from Scotch thistle.

    Science.gov (United States)

    Móricz, Ágnes M; Krüzselyi, Dániel; Alberti, Ágnes; Darcsi, András; Horváth, Györgyi; Csontos, Péter; Béni, Szabolcs; Ott, Péter G

    2017-11-17

    The antibacterial profiling of Onopordum acanthium L. leaf extract and subsequent targeted identification of active compounds is demonstrated. Thin-layer chromatography (TLC) and off-line overpressured layer chromatography (OPLC) coupled with direct bioautography were utilized for investigation of the extract against eight bacterial strains including two plant and three human pathogens and a soil, a marine and a probiotic human gut bacteria. Antibacterial fractions obtaining infusion-transfusion OPLC were transferred to HPLC-MS/MS analysis that resulted in the characterization of three active compounds and two of them were identified as, linoleic and linolenic acid. OPLC method was adopted to preparative-scale flash chromatography for the isolation of the third active compound, which was identified after a further semi-preparative HPLC purification as the germacranolide sesquiterpene lactone onopordopicrin. Pure onopordopicrin exhibited antibacterial activity that was specified as minimal inhibitory concentration in the liquid phase as well. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Le dépôt de diamant en couche mince et ses applications Thin-Layer Diamond Depositing and Its Applications

    Directory of Open Access Journals (Sweden)

    Bertrand A.

    2006-11-01

    Full Text Available Nous avons cherché à faire le point sur la fabrication de couches minces de diamant qui, après avoir été très étudiée aux États-Unis vers la fin des années 1950, a fait l'objet d'une percée technologique soviétique en 1977. Celle-ci utilise l'effet solvant de l'hydrogène mélangé à un peu de méthane. Transformé en hydrogène atomique par décharge électrique, il interdit le dépôt de graphite et par conséquent permet seulement celui du diamant. Ce résultat est riche d'applications prometteuses en mécanique, en optique, en électronique. . . et constitue un élément clé pour la recherche spatiale. Les Japonais ont mis cinq ans pour réagir et les Américains cinq autres années. Mais ces derniers espèrent refaire leur retard grâce au programme Diamond Technology Initiative établi dans le cadre de l'initiative de Défense Stratégique (Guerre des Étoiles. Les retombées de ces travaux devraient concerner l'industrie pétrolière (paliers, trépans, capteurs en milieu extrême. This article reviews the depositing of diamond thin layers. After much research had been done on this technique in the United States in the late 1950s, a technological breakthrough was made by the Soviets in 1977. This breakthrough uses the solventeffect of hydrogen mixed with a bit of methane. This is transformed into atomic hydrogen by an electric discharge, thus preventing graphite from being deposited and hence enabling only diamond to be deposited. This achievement has a wealth of promising applications in mechanics, optics, electronics, etc. It is also a key element for space research. The Japanese took five years to react and the Americans another five years. But these latter hope to make up for lost time with the Diamond Technology Initiativepromoted within the framework of the Strategic Defense Initiative ( star wars . The fallouts from this research should involve the petroleum industry (bearings, drill bits, sensors in extreme

  10. Protein and virus-like particle adsorption on perfusion chromatography media.

    Science.gov (United States)

    Wu, Yige; Simons, Jared; Hooson, Sarah; Abraham, Dicky; Carta, Giorgio

    2013-07-05

    The structural and protein adsorption characteristics of the perfusion chromatography matrix POROS(®) HS 50 are determined. Transmission electron microscopy shows a broad distribution of pore sizes with 100-500nm through-pores transecting a network of much smaller pores formed by aggregates of microgranules about 100nm in size. Dextran standards, proteins, and virus-like particles (VLPs) show size-exclusion behavior consistent with such a bimodal distribution of pore sizes. For non-binding conditions, the trends in height equivalent to a theoretical plate (HETP) as a function of mobile phase velocity and molecular size are consistent with perfusion suggesting that a fraction of the mobile phase between 0.0005 and 0.0008 flows through the particles. This small fraction provides little or no enhancement of intraparticle mass transfer for relatively small proteins (lysozyme and IgG) even at 1000cm/h, but can contribute substantially to transport for large proteins (thyroglobulin) and VLPs. Intraparticle concentration profiles during transient adsorption are determined by confocal microscopy in batch and flow systems. The profiles are spherically symmetrical indicating a dominance of diffusion for smaller proteins in both batch and flow systems but become highly asymmetrical and skewed in the direction of flow for thyroglobulin at 1000cm/h. Estimates of the convective enhancement of intraparticle transport for these conditions based on the confocal measurements are consistent with estimates of the intraparticle Peclet number and previously published models. Adsorption of VLPs, however, was found to be confined to a thin layer on the outer surface of the particles indicting that bound VLPs block access to the underlying pore network and suggesting that pores larger than those present on the resin studies are needed to take advantage of the effects of perfusion for the adsorption of large VLPs. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Biological Fingerprinting of Herbal Samples by Means of Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    Łukasz Cieśla

    2012-01-01

    Full Text Available Biological chromatographic fingerprinting is a relatively new concept in the quality control of herbal samples. Originally it has been developed with the application of HPLC, and recently herbal samples' biological profiles have been obtained by means of thin-layer chromatography (TLC. This paper summarizes the application of liquid chromatographic techniques for the purpose of biological fingerprint analysis (BFA of complex herbal samples. In case of biological TLC fingerprint, which is a relatively novel solution, perspectives of its further development are outlined in more detail. Apart from already published data, some novel results are also shown and briefly discussed. The paper aims at drawing scientists' attention to the unique solutions offered by biological fingerprint construction.

  12. Standardization of Unani polyherbal formulation, Qurse-e-Hummaz: A comprehensive approach

    Directory of Open Access Journals (Sweden)

    Y T Kamal

    2016-01-01

    Full Text Available Background: An increase in the awareness about the advantages of the traditional system of medicines has led to the commercialization of the formulations used for the treatments. Manufacture of these medicines to meet this increasing demand has resulted in a decline in their quality, primarily due to a lack of adequate regulations pertaining to this sector of medicine. Hence, it is necessary to come up with a systematic approach to develop well-designed methodologies for the standardization of polyherbal formulations which are used in traditional systems of medicine. Materials and Methods: Qurs-e-Hummaz formulations were prepared by a qualified “Hakim” (Unani medical practitioner of Faculty of Unani Medicine, Hamdard University, as per the formula and instruction given in National Formulary of Unani Medicine. Results: Various quality control parameters such as organoleptic evaluations (color, odor, taste, and consistency, physicochemical evaluations (loss on drying, disintegration time, moisture content, total ash, acid insoluble ash, water soluble ash, pH of 1 and 10% solution, extractive values, water soluble matter, alcohol-soluble matter, and total phenolic content and thin layer chromatography fingerprint profiling have been carried out in triplicate. The evaluation of contaminants such as heavy metals, aflatoxins, pesticide residues, and microbial contamination has also been carried out in the formulation. Conclusion: Help in maintaining the quality and batch to batch consistency of many important polyherbal formulations.

  13. Comparison of chromatography systems for radiochemical purity determination of lyophilized reagents labeled with technetium-99m

    Energy Technology Data Exchange (ETDEWEB)

    Monteiro, Elisiane G.; Almeida, Erika V.; Ramos, Marcelo P.S.; Alves, Edson V.; Benedetti, Stella; Mengatti, Jair; Fukumori, Neuza T.O.; Matsuda, Margareth M.N., E-mail: elisianegodoy@terra.com.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2009-07-01

    A variety of lyophilized reagents (LR) labeled with {sup 99m}Tc has been developed for determining organ function or assessing disease status by imaging methods. Usually, the quality of the radiopharmaceutical preparations is evaluated by paper chromatography (PC), thin layer chromatography (TLC), instant thin layer chromatography silica gel (ITLC-SG), high performance liquid chromatography (HPLC) on reverse-phase columns and capillary electrophoresis (CE). PC and TLC have been applied due to the low cost and short time in the determination of pertechnetate ({sup 99m}TcO{sub 4}-) and technetium dioxide ({sup 99m}TcO{sub 2}). The present study reports the comparison between PC and TLC chromatographic methods for determination of the radiochemical purity of LR labeled with {sup 99m}Tc from IPEN-CNEN/SP (Brazil). PC was performed with Whatman 3MM/1MM paper chromatography strips and TLC with ITLC-SG sheets or reversed phase (RP). RP was used only for ECD. Although the radioactivity profile of the separation of the species on both stationary phases was satisfactory, the difference in results for % {sup 99m}TcO{sub 4}- and {sup 99m}TcO{sub 2} was up to 4.2 % using PC for ECD and PYP. ITLC supports gave better resolution than conventional PC supports for these products. In ECD analysis, the comparison was performed between RP and ITLC-SG stationary phases for determination of {sup 99m}TcO{sub 4}-, {sup 99m}TcO{sub 2} and other impurities. It was observed that the sheet length as described in the United States Pharmacopoeia was not sufficient for a good separation of the product and the impurities. The results showed that there were not significant differences between PC and TLC chromatographic stationary phases are going to be accomplished. (author)

  14. Depth profiling of fluorine-doped diamond-like carbon (F-DLC) film: Localized fluorine in the top-most thin layer can enhance the non-thrombogenic properties of F-DLC

    Energy Technology Data Exchange (ETDEWEB)

    Hasebe, Terumitsu [Center for Science of Environment, Resources and Energy, Keio University Faculty of Science and Technology, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama, Kanagawa 223-8522 (Japan); Department of Radiology, Tachikawa Hospital, 4-2-22, Nishiki-cho, Tachikawa, Tokyo 190-8531 (Japan)], E-mail: teru_hasebe@hotmail.com; Nagashima, So [Center for Science of Environment, Resources and Energy, Keio University Faculty of Science and Technology, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama, Kanagawa 223-8522 (Japan); Kamijo, Aki [Department of Transfusion Medicine, the University of Tokyo Hospital, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8655 (Japan); Yoshimura, Taichi; Ishimaru, Tetsuya; Yoshimoto, Yukihiro; Yohena, Satoshi; Kodama, Hideyuki; Hotta, Atsushi [Center for Science of Environment, Resources and Energy, Keio University Faculty of Science and Technology, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama, Kanagawa 223-8522 (Japan); Takahashi, Koki [Department of Transfusion Medicine, the University of Tokyo Hospital, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8655 (Japan); Suzuki, Tetsuya [Center for Science of Environment, Resources and Energy, Keio University Faculty of Science and Technology, 3-14-1 Hiyoshi, Kohoku-ku, Yokohama, Kanagawa 223-8522 (Japan)

    2007-12-03

    Fluorine-doped diamond-like carbon (F-DLC) has recently drawn a great deal of attention as a more non-thrombogenic coating than conventional DLC for blood-contacting medical devices. We conducted quantitative depth profiling of F-DLC film by X-ray photoelectron spectroscopy (XPS) in order to elucidate the effects of fluorine and fluorine distribution in F-DLC film in connection with the prevention of surface blood adhesion. F-DLC films were prepared on silicon substrates using the radio frequency plasma enhanced chemical vapor deposition method, and the thickness of films was {approx} 50 nm. 50-nm-thick F-DLC film samples were etched at 10-nm thickness intervals using argon plasma, and each surface was examined by XPS. Thereafter, each etched film layer was incubated with platelet-rich plasma isolated from human whole blood, and the platelet-covered area per unit area was evaluated for each surface. XPS spectra showed the localization of doped fluorine in the top-most thin layer of the film. Platelet-covered areas represented progressively larger portions of the surfaces of deeper etched layers, corresponding to the decreasing fluorine content in such sample surfaces. These results indicate that the localized fluorine in the top-most thin layer is one of the key factors in the promotion of the non-thrombogenicity of F-DLC film.

  15. A practical strategy for using miniature chromatography columns in a standardized high-throughput workflow for purification development of monoclonal antibodies.

    Science.gov (United States)

    Welsh, John P; Petroff, Matthew G; Rowicki, Patricia; Bao, Haiying; Linden, Thomas; Roush, David J; Pollard, Jennifer M

    2014-01-01

    The emergence of monoclonal antibody (mAb) therapies has created a need for faster and more efficient bioprocess development strategies in order to meet timeline and material demands. In this work, a high-throughput process development (HTPD) strategy implementing several high-throughput chromatography purification techniques is described. Namely, batch incubations are used to scout feasible operating conditions, miniature columns are then used to determine separation of impurities, and, finally, a limited number of lab scale columns are tested to confirm the conditions identified using high-throughput techniques and to provide a path toward large scale processing. This multistep approach builds upon previous HTPD work by combining, in a unique sequential fashion, the flexibility and throughput of batch incubations with the increased separation characteristics for the packed bed format of miniature columns. Additionally, in order to assess the applicability of using miniature columns in this workflow, transport considerations were compared with traditional lab scale columns, and performances were mapped for the two techniques. The high-throughput strategy was utilized to determine optimal operating conditions with two different types of resins for a difficult separation of a mAb monomer from aggregates. Other more detailed prediction models are cited, but the intent of this work was to use high-throughput strategies as a general guide for scaling and assessing operating space rather than as a precise model to exactly predict performance. © 2014 American Institute of Chemical Engineers.

  16. Implementation of 350-2500 nm diffuse reflectance spectroscopy and High-Performance Thin-Layer Chromatography to rapidly assess manufacturing consistency and quality of cotrimoxazole tablets in Tanzania.

    Science.gov (United States)

    Kaale, Eliangiringa; Hope, Samuel M; Jenkins, David; Layloff, Thomas

    2016-01-01

    To assess the quality of cotrimoxazole tablets produced by a Tanzanian manufacturer by a newly instituted quality assurance programme. Tablets underwent a diffuse reflectance spectroscopy procedure with periodic quality assessment confirmation by assay and dissolution testing using validated HPTLC techniques (including weight variation and disintegration evaluations). Based on results from the primary test methods, the first group of product was 99% compliance. This approach provides a model for rapidly assuring product quality of future procurements of other products that is more cost-effective than traditional pharmaceutical testing techniques. © 2015 John Wiley & Sons Ltd.

  17. Systematic evaluation of the root cause of non-linearity in liquid chromatography/tandem mass spectrometry bioanalytical assays and strategy to predict and extend the linear standard curve range.

    Science.gov (United States)

    Yuan, Long; Zhang, Duxi; Jemal, Mohammed; Aubry, Anne-Francoise

    2012-06-30

    The linear range of a liquid chromatography/tandem mass spectrometry (LC/MS/MS) bioanalytical assay is typically about three orders of magnitude. A broader standard curve range is favored since it can significantly reduce the time, labor and potential errors related to sample dilution - one of the bottlenecks in sample analysis. Using quadratic regression to fit the standard curve can, to a certain degree, extend the dynamic range. However, the use of a quadratic regression is controversial, particularly in regulated bioanalysis. A number of compounds, with different physicochemical properties and ionization efficiencies, were evaluated to understand the cause of the non-linear behavior of the standard curve. The standard curve behavior is primarily associated with the absolute analyte response but not the analyte concentration, the properties of the analyte, or the nature of the matrix when a stable-isotope-labeled internal standard (SIL-IS) is used. For all the test compounds, a non-linear curve was observed when signals exceeded a certain response, which depends on the detector used in the mass spectrometer. With typical API4000 instruments used for the experiments, this critical response level was determined to be ~1 E+6 counts per second (cps) and it was successfully used to predict the linear ranges for the test compounds. By simultaneously monitoring two selective reaction monitoring (SRM) channels of different intensity and using SIL-IS, a linear range of five orders of magnitude was achieved. In this work, the root cause of the non-linear behavior of the standard curve when using a SIL-IS was investigated and identified. Based on the findings, an improved multiple SRM channels approach was proposed and successfully applied to obtain a linear dynamic range of five orders of magnitude for one test compound. This approach may work particularly well for LC/MS/MS bioanalytical assay of dried blood spot (DBS) samples, for which a direct dilution is cumbersome

  18. Compensation of matrix effects in gas chromatography-mass spectrometry analysis of pesticides using a combination of matrix matching and multiple isotopically labeled internal standards.

    Science.gov (United States)

    Tsuchiyama, Tomoyuki; Katsuhara, Miki; Nakajima, Masahiro

    2017-11-17

    In the multi-residue analysis of pesticides using GC-MS, the quantitative results are adversely affected by a phenomenon known as the matrix effect. Although the use of matrix-matched standards is considered to be one of the most practical solutions to this problem, complete removal of the matrix effect is difficult in complex food matrices owing to their inconsistency. As a result, residual matrix effects can introduce analytical errors. To compensate for residual matrix effects, we have developed a novel method that employs multiple isotopically labeled internal standards (ILIS). The matrix effects of ILIS and pesticides were evaluated in spiked matrix extracts of various agricultural commodities, and the obtained data were subjected to simple statistical analysis. Based on the similarities between the patterns of variation in the analytical response, a total of 32 isotopically labeled compounds were assigned to 338 pesticides as internal standards. It was found that by utilizing multiple ILIS, residual matrix effects could be effectively compensated. The developed method exhibited superior quantitative performance compared with the common single-internal-standard method. The proposed method is more feasible for regulatory purposes than that using only predetermined correction factors and is considered to be promising for practical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Evaluation of the impact of matrix effect on quantification of pesticides in foods by gas chromatography-mass spectrometry using isotope-labeled internal standards.

    Science.gov (United States)

    Yarita, Takashi; Aoyagi, Yoshie; Otake, Takamitsu

    2015-05-29

    The impact of the matrix effect in GC-MS quantification of pesticides in food using the corresponding isotope-labeled internal standards was evaluated. A spike-and-recovery study of nine target pesticides was first conducted using paste samples of corn, green soybean, carrot, and pumpkin. The observed analytical values using isotope-labeled internal standards were more accurate for most target pesticides than that obtained using the external calibration method, but were still biased from the spiked concentrations when a matrix-free calibration solution was used for calibration. The respective calibration curves for each target pesticide were also prepared using matrix-free calibration solutions and matrix-matched calibration solutions with blank soybean extract. The intensity ratio of the peaks of most target pesticides to that of the corresponding isotope-labeled internal standards was influenced by the presence of the matrix in the calibration solution; therefore, the observed slope varied. The ratio was also influenced by the type of injection method (splitless or on-column). These results indicated that matrix-matching of the calibration solution is required for very accurate quantification, even if isotope-labeled internal standards were used for calibration. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Speciation of eight arsenic compounds in human urine by high performance liquid chromatography with inductively coupled plasma mass spectrometric detection using antimonate for internal chromatographic standardization

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Pritzl, G.; Hansen, S. H.

    1993-01-01

    and dimethylarsinate and the cations arsenobetaine, trimethylarsine oxide, arsenocholine and the tetramethylarsonium ion. Hexahydroxyantimonate(III) was co-chromatographed with the arsenic anions but detected at m/z 121 and used as an internal standard for their qualitative analysis. Arsenite was prone to oxidation...

  1. Quantification of endogenous metabolites by the postcolumn infused-internal standard method combined with matrix normalization factor in liquid chromatography-electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Liao, Hsiao-Wei; Chen, Guan-Yuan; Wu, Ming-Shiang; Liao, Wei-Chih; Tsai, I-Lin; Kuo, Ching-Hua

    2015-01-02

    Quantification of endogenous metabolites has enabled the discovery of biomarkers for diagnosis and provided for an understanding of disease etiology. The standard addition and stable isotope labeled-internal standard (SIL-IS) methods are currently the most widely used approaches to quantifying endogenous metabolites, but both have some limitations for clinical measurement. In this study, we developed a new approach for endogenous metabolite quantification by the postcolumn infused-internal standard (PCI-IS) method combined with the matrix normalization factor (MNF) method. MNF was used to correct the difference in MEs between standard solution and biofluids, and PCI-IS additionally tailored the correction of the MEs for individual samples. Androstenedione and testosterone were selected as test articles to verify this new approach to quantifying metabolites in plasma. The repeatability (n=4 runs) and intermediate precision (n=3 days) in terms of the peak area of androstenedione and testosterone at all tested concentrations were all less than 11% relative standard deviation (RSD). The accuracy test revealed that the recoveries were between 95.72% and 113.46%. The concentrations of androstenedione and testosterone in fifty plasma samples obtained from healthy volunteers were quantified by the PCI-IS combined with the MNF method, and the quantification results were compared with the results of the SIL-IS method. The Pearson correlation test showed that the correlation coefficient was 0.98 for both androstenedione and testosterone. We demonstrated that the PCI-IS combined with the MNF method is an effective and accurate method for quantifying endogenous metabolites. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. Validated thin-layer chromatographic method for the identification and monitoring of the effect of the extraction method on the yield and phytochemical constituents of Egyptian Withania somnifera leaves.

    Science.gov (United States)

    Mahrous, Rahma S R; Fathy, Hoda M; Abu El-Khair, Rasha M; Omar, Abdallah A

    2018-01-01

    A sensitive, reliable, simple and rapid thin-layer chromatographic method has been developed for routine analysis of withanolide S content for the purpose of quality control assessment of chemotype III of Withania somnifera. The new method was used first to compare the accumulation of withanolide S in different parts of the plant, which was found to be the highest in the leaves extract (0.21% w/w). Second, to investigate different extraction parameters that improve the extraction efficiency of withanolides from the leaves using conventional and ultrasound-assisted extraction methods. The extraction efficiency was expressed via total withanolide content and withanolide S content. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Development and Validation of High Performance Thin-Layer Chromatographic Method for Determination of α-Mangostin in Fruit Pericarp of Mangosteen Plant (Garcinia mangostana L. using Ultraviolet – Visible Detection

    Directory of Open Access Journals (Sweden)

    Himanshu Misra

    2009-10-01

    Full Text Available A simple, fast and precise quantitative high performance thin-layer chromatographic method has been developed for quantitative estimation of α-mangostin in fruit pericarp of Garcinia mangostana L. (Hypericaceae. Best solvent for extraction of a-mangostin optimized after screening with five solvents under same conditions using hot solid-liquid extraction through soxhlet apparatus. Methanol and chloroform gave highest and second highest recovery of a-mangostin, respectively. Plates were developed in chloroform-methanol in the ratio of 27-3 (v/v. Post-chromatographic derivatization performed using anisaldehyde-sulphuric acid reagent and scanned at 382 nm in ultraviolet-visible mode. The developed method was found to be linear in the range 1.0 to 5.0 mg spot-1, limits of detection and quantitation were 150 and 450 ng spot-1. The developed method was validated in terms of system suitability, specificity and robustness.

  4. Determination of bitter orange alkaloids in dietary supplement Standard Reference Materials by liquid chromatography with atmospheric-pressure ionization mass spectrometry.

    Science.gov (United States)

    Putzbach, Karsten; Rimmer, Catherine A; Sharpless, Katherine E; Wise, Stephen A; Sander, Lane C

    2007-09-01

    A liquid chromatographic atmospheric-pressure ionization electrospray mass spectrometry (LC-API-ES-MS) method has been developed for the determination of five bitter orange alkaloids (synephrine, octopamine, n-methyltyramine, tyramine, and hordenine) in bitter orange-containing dietary supplement standard reference materials (SRMs). The materials represent a variety of natural, extracted, and processed sample matrices. Two extraction techniques were evaluated: pressurized-fluid extraction (PFE) and sonication extraction. The influence of different solvents, extraction temperatures, and pH were investigated for a plant material and a processed sample. The LC method uses a new approach for the separation of highly polar alkaloids. A fluorinated, silica-based stationary phase separated the five alkaloids and the internal standard terbutaline in less than 20 min. This method enabled the determination of the dominant alkaloid synephrine and other minor alkaloids in a variety of dietary supplement SRMs.

  5. Application of Doehlert uniform shell designs for selecting optimal amounts of internal standards in the analysis of prostaglandins and leukotrienes by liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Araujo, Pedro; Janagap, Steve; Holen, Elisabeth

    2012-10-19

    A protocol for the analysis of multiple prostaglandins and leukotrienes in cell culture media by using multiple internal standards was validated. A two-factor Doehlert design was used to determine the behaviour of the relationship analyte/internal standard (namely: PGE2/PGE2-d4, PGE3/PGE2-d4, LTB4/LTB4-d4 and LTB5/LTB4-d4) and to select the optimal amounts of deuterated internal standards for quantifying simultaneously the prostaglandins and leukotrienes in cell culture media by LC-MS/MS. The selection of optimal amounts of internal standards was based on mathematical models that allow visualizing concentration regions where the response factors remain constant over a wide range of analytical concentrations. The linearity of the calibration curves for each analyte at the optimal levels suggested by the mathematical models was statistically confirmed by means of the ratio lack-of-fit to pure error. The validated protocol was successfully applied in the simultaneous quantification of pro- and anti-inflammatory eicosanoids in stimulated cod head kidney cell culture media. The two-factor Doehlert design has permitted to estimate the experimental response as a function of six variables (PGE2, PGE3, LTB4, LTB5, PGE2-d4 and LTB4-d4) which represents a substantial reduction of resources, time and experiments of approximately 84% (7×3 experiments) when compared with the full six-factor Doehlert design (43×3 experiments). Copyright © 2012 Elsevier B.V. All rights reserved.

  6. Electrophoretically mediated microanalysis for simultaneous on-capillary derivatization of standard amino acids followed by micellar electrokinetic capillary chromatography with laser-induced fluorescence detection.

    Science.gov (United States)

    Celá, Andrea; Mádr, Aleš; Glatz, Zdeněk

    2017-05-26

    Amino acids are crucial compounds involved in most biochemical processes essential for life. Since their dynamic turnover reflects the actual physiology of the cell/organism, a turnover assessment may provide valuable information related to multiple physiological and pathophysiological conditions. The sensitive determination of amino acids is predominantly associated with their derivatization which might be laborious, time-consuming and difficult to standardize. However, capillary electrophoresis offers the automatic injection and mixing of reactants, incubation of the reaction mixture, separation and detection of the reaction products in one on-capillary procedure. Among the on-capillary mixing strategies, electrophoretically mediated microanalysis (EMMA) is superior in terms of mixing efficiency. In this paper, we present an optimization of EMMA for the simultaneous derivatization of standard amino acids by naphthalene-2,3-dicarboxaldehyde/NaCN and its application to targeted human embryo metabolomics. For such a purpose, novel separation conditions were developed involving the background electrolyte, comprised of 73mM sodium dodecyl sulfate, 6.7 % (v/v) 1-propanol, 0.5mM (2-hydroxypropyl)-β-cyclodextrin and 135mM boric acid/sodium hydroxide buffer (pH 9.00). Finally, the optimized EMMA was compared to a fundamentally different mixing strategy, namely the transverse diffusion of laminar flow profiles, and proved to be also suitable for human plasma analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. TLC-MS versus TLC-LC-MS fingerprints of herbal extracts. Part III. Application of the reversed-phase liquid chromatography systems with C18 stationary phase.

    Science.gov (United States)

    Sajewicz, Mieczysław; Staszek, Dorota; Natic, Maja; Waksmundzka-Hajnos, Monika; Kowalska, Teresa

    2011-08-01

    In the previous paper from this series, we proposed mass spectrometric fingerprinting of complex botanical samples upon the examples of the pharmacologically important phenolic acids and flavonoids selectively extracted from Salvia lavandulifolia. In this study, we explore fingerprinting efficiency with a novel two-dimensional analytical system composed of the reversed-phase thin-layer chromatography and the reversed-phase high performance liquid chromatography with mass spectrometric detection (2D RP-TLC-RP-LC-MS). We also compare its efficiency with that of the one-dimensional analytical system (the reversed-phase thin-layer chromatography with mass spectrometric detection; 1D RP-TLC-MS). As our present study is basically focused on the method development, we considered it as justified to carry out our comparison with the phenolic acid extracts selectively derived from the Salvia lavandulifolia species, similar as it was done in Part II from this series. Upon the results obtained, it was established that the 1D RP-TLC-MS mode and the 2D RP-TLC-RP-LC-MS mode can be applied to fingerprinting of herbal extracts, and that the 2D RP-TLC-RP-LC mode can provide a more abundant information than that originating from the 1D RP-TLC mode.

  8. Analytical speciation of mercury in fish tissues by reversed phase liquid chromatography-inductively coupled plasma mass spectrometry with Bi(3+) as internal standard.

    Science.gov (United States)

    Santoyo, María Maldonado; Figueroa, Julio Alberto Landero; Wrobel, Kazimierz; Wrobel, Katarzyna

    2009-08-15

    In this work, the quantification of two mercury species (Hg(2+) and CH(3)Hg(+)) in fish tissues has been revisited. The originality of our approach relies on the use of Bi(3+) as internal standard (IS) and on the modification of typical extraction conditions. The IS (125 microl, 1000 microg l(-1) Bi(3+)) was added to the aliquot of fresh fish tissue (400-500 mg). A high-speed blender and ultrasound-assisted homogenization/extraction was carried out in the presence of perchloric acid (1.5 ml, 0.6 mol l(-1)), l-cysteine (500 microl, 0.75 mol l(-1)) and 500 microl toluene:methanol (1:1). Perchloric acid was used for protein denaturation and precipitation, toluene helped to destroy lipid structures potentially sequestering CH(3)Hg(+), L-cysteine was used to form water-soluble complexes with Bi(3+), Hg(2+) and CH(3)Hg(+). The excess of perchloric acid was eliminated by addition of potassium hydroxide (pH 5 with acetic acid). The obtained extract, was diluted with the mobile phase (1:1) and introduced (20 microl) to the reversed phase HPLC-ICP-MS system. The separation was achieved by isocratic elution (2.5 mmol l(-1) cysteine, 12.5 mmol l(-1) (NH(4))(2)HPO(4), 0.05% triethylamine, pH 7.0:methanol (96:4)) at a flow rate 0.6 ml min(-1). Column effluent was on-line introduced to ICP-MS for specific detection of (202)Hg, (200)Hg and (209)Bi. Analytical signal was defined as the ratio between (202)Hg/(209)Bi peak areas. The detection limits evaluated for Hg(2+) and CH(3)Hg(+) were 0.8 and 0.7 microg l(-1). Recovery of the procedure, calculated as the sum of species concentrations found in the sample with respect to total ICP-MS-determined Hg was 91.9% for king mackerel muscle and 89.5% for red snapper liver. In the standard addition experiments, the recovery results were 98.9% for Hg(2+) and 100.6% for CH(3)Hg(+). It should be stressed that the use of Bi(3+) as IS enabled to improve analytical performance by compensating for incomplete extraction and for imprecision of

  9. Simultaneous multiple mycotoxin quantification in feed samples using three isotopically labeled internal standards applied for isotopic dilution and data normalization through ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry.

    Science.gov (United States)

    Jackson, Lewis C; Kudupoje, Manoj B; Yiannikouris, Alexandros

    2012-12-15

    Mycotoxins are typically present in grain and are also concentrated in distillers dried grains with solubles (DDGS), common feed ingredients for food animals. The diversity of mycotoxins and feed matrices has made the routine detection and quantification of mycotoxins in feed both complex and prohibitively expensive. Ultra-performance liquid chromatography/electrospray ionization triple quadrupole detection (UPLC/ESI-TQD) (tandem mass spectrometry, MS/MS) with (13) C-labeled isotopic dilution was used to analyze internal standard isotopologues of three mycotoxin molecules, as well as 29 other structurally differing mycotoxin molecules from four common feed matrices: corn, wheat, barley, or DDGS. Mycotoxins were extracted via a single-step procedure using a mixture of acetonitrile/water/formic acid. Labeled isotopologues were used as a surrogate to account for extraction quality and as internal standards for the evaluation of the feed matrix signal suppression/enhancement (SSE) contributed by each mycotoxin and by each matrix. The SSE was corrected by matrix-matched calibration with blank certified reference feed material. The limits of detection for individual mycotoxins in buffer ranged from 0.01 to 206.7 µg/mL but could increase by up to four times depending on the matrix effect. The accuracy and precision were enhanced by the use of isotopically labeled standards. The recoveries were somewhat negatively affected by the SSE contributed by each matrix. Each mycotoxin was successfully detected and assigned to one of four SSE categories: high (-66%), intermediate (-48%), low (-19%) signal suppression and signal enhancement (> +300%). An improved LC/MS method was validated, which offers a practical and economical means for large-scale detection and quantification of multiple mycotoxins in common animal-feed matrices, including DDGS. Copyright © 2012 John Wiley & Sons, Ltd.

  10. Separation method of uranium and plutonium by using Extraction Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Inoue, Shin-ichi; Shinohara, Toshihisa; Sato, Yoshihiro; Hatakenaka, Teruo; Nidaira, Kazuo; Tokoro, Youichi [Nuclear Material Control Center, Tokyo (Japan)

    1997-12-31

    In order to test adaptation of Extraction Chromatography to routine analysis of U/Pu, the comparison of anion-exchange separation method used in our laboratory with TOPO extraction chromatography used in IAEA-SAL and the extraction chromatography using TEVA{center_dot}Spec.regin were made. Good results with recovery and analytical time were obtained for Extraction Chromatography. Further experiments must await on standardization of adsorbent, cost reduction and simplification of procedure. (author)

  11. A thin layer electrochemical cell for disinfection of water contaminated with Staphylococcus aureus Uma célula eletroquímica de camada delgada para desinfecção de água contaminada com Staphylococcus aureus

    Directory of Open Access Journals (Sweden)

    Isabel C. P. Gusmão

    2009-09-01

    Full Text Available A thin layer electrochemical cell was tested and developed for disinfection treatment of water artificially contaminated with Staphylococcus aureus. Electrolysis was performed with a low-voltage DC power source applying current densities of 75 mA cm-2(3 A or 25 mA cm-2 (1 A. A dimensionally stable anode (DSA of titanium coated with an oxide layer of 70%TiO2 plus 30%RuO2 (w/w and a 3 mm from a stainless-steel 304 cathode was used in the thin layer cell. The experiments were carried out using a bacteria suspension containing 0.08 M sodium sulphate with chloridefree to determine the bacterial inactivation efficacy of the thin layer cell without the generation of chlorine. The chlorine can promote the formation of trihalomethanes (THM that are carcinogenic. S. aureus inactivation increased with electrolysis time and lower flow rate. The flow rates used were 200 or 500 L h-1. At 500 L h-1 and 75 mA cm -2 the inactivation after 60 min was about three logs of decreasing for colony forming units by mL. However, 100% inactivation for S. aureus was observed at 5.6 V and 75 mA cm-2 after 30 min. Thus, significant disinfection levels can be achieved without adding oxidant substances or generation of chlorine in the water.Uma célula eletroquímica de camada delgada foi utilizada e desenvolvida para a desinfecção de água contaminada artificialmente com Staphylococcus aureus. A eletrólise foi executada com uma fonte de corrente direta utilizando 75 mA cm-2 (3 A ou 25 mA cm-2 (1 A. Um anodo dimensionalmente estável (DSA de titânio revestido com uma camada do óxido de 70%TiO2 e 30%RuO2 (w/w e distanciado por 3 milímetros de um catodo de aço inoxidável 304 foi utilizado para gerar uma camada delgada de suspensão bacteriana passando pela célula de camada delgada. As suspensões utilizadas eram feitas apenas com Na2SO4 0,08 M e livre de íons cloretos de forma a inativar as células bacterianas no tratamento eletroquímico sem a geração de cloro

  12. Use of quartz crystal nanobalance to study the binding and stabilization of albumin and doxycycline on a thin layer of hydroxyapatite

    Science.gov (United States)

    Victor, Sunita Prem; Sharma, Chandra P.; Sreenivasan, K.

    2011-12-01

    This study reports the use of quartz crystal nanobalance (QCN) to study the adsorption of two model molecules namely albumin and doxycycline by hydroxyapatite (HA). The work focuses on the deposition of a stable coating of HA on the quartz crystal, modification of the coating using doxycycline and its subsequent effects on albumin adsorption. The uniformity and thickness of the HA coating has been studied using atomic force microscopy (AFM). The functional groups to ascertain the presence of the selected moieties have been characterized by Raman spectroscopy. The results indicate that the mass of albumin deposited on the surface of the HA coated quartz crystal functionalized with doxycycline shows a substantial increase when compared to the standard HA coated quartz crystal. The adsorbed albumin has also been found to be retained for an enhanced period of time. This surface immobilization of doxycycline and subsequent albumin adsorption seem to be a promising approach to confer biomaterials with antithrombogenic and antibacterial surfaces.

  13. Use of quartz crystal nanobalance to study the binding and stabilization of albumin and doxycycline on a thin layer of hydroxyapatite

    Energy Technology Data Exchange (ETDEWEB)

    Victor, Sunita Prem [Biosurface Technology Division, Biomedical Technology Wing, Sree Chitra Tirunal Institute for Medical Sciences and Technology, Trivandrum 695012, Kerala (India); Sharma, Chandra P., E-mail: sharmacp@sctmist.ac.in [Biosurface Technology Division, Biomedical Technology Wing, Sree Chitra Tirunal Institute for Medical Sciences and Technology, Trivandrum 695012, Kerala (India); Sreenivasan, K. [Biosurface Technology Division, Biomedical Technology Wing, Sree Chitra Tirunal Institute for Medical Sciences and Technology, Trivandrum 695012, Kerala (India); Laboratory for Polymer Analysis, Biomedical Technology Wing, Sree Chitra Tirunal Institute for Medical Sciences and Technology, Trivandrum 695012, Kerala (India)

    2011-12-15

    This study reports the use of quartz crystal nanobalance (QCN) to study the adsorption of two model molecules namely albumin and doxycycline by hydroxyapatite (HA). The work focuses on the deposition of a stable coating of HA on the quartz crystal, modification of the coating using doxycycline and its subsequent effects on albumin adsorption. The uniformity and thickness of the HA coating has been studied using atomic force microscopy (AFM). The functional groups to ascertain the presence of the selected moieties have been characterized by Raman spectroscopy. The results indicate that the mass of albumin deposited on the surface of the HA coated quartz crystal functionalized with doxycycline shows a substantial increase when compared to the standard HA coated quartz crystal. The adsorbed albumin has also been found to be retained for an enhanced period of time. This surface immobilization of doxycycline and subsequent albumin adsorption seem to be a promising approach to confer biomaterials with antithrombogenic and antibacterial surfaces.

  14. Multielement XRF analysis of mono- and polycrystal microsamples by the thin layer method. Determination of Ni, Cu, Zn, Ga, Cd, Cr, Se

    Energy Technology Data Exchange (ETDEWEB)

    Jurczyk, J.; Sitko, R.; Buhl, F. [Institute of Chemistry, Silesian University, Katowice (Poland)

    1998-12-31

    0.5 mg of the investigated disintegrated mono- or polycrystals of M/N/Cr/Se where M, N - Cu, Zn, Ni, Ga, Cd, Co, In and others are spread on the substrate (a Milipore filter glued on the glass plate by means of two-sided adhesive type), digested by spreading concentrated nitric and hydrochloric acid and dried under IR heater. A standard graph is performed on the basis of synthetic standard samples with the same chemical composition but varied weights: 0.1-1.2 mg, prepared by transferring a multielement solution on the substrate by means of micropipette. Instrumental conditions: a sequential wave-dispersive spectrometer, X-ray tube with a W anode, 50 kV, 40 mA, K{sub {alpha}} lines; LiF 200 crystal, flow or scintillation counter or their combination depending on the element, vacuum measurements, rotation of sample, 40 s counting time. Statistical parameters: detection limits for 0.5 mg samples: Cu 0.041-0.048% (0.21-0.24 {mu}g), Zn 0.024-0.034% (0.12-0.17 {mu}g), Ga 0.079-0.102% (0.40-0.51 {mu}g), Ni 0.016% (0.08 {mu}g), Cd 1.9% (9.5 {mu}g), Cr 0.018-0.030% (0.09-0.15 {mu}g), Se 0.108-0.151% (0.54-0.76 {mu}g), linear correlation coefficients R>0.99. (author) 26 refs, 7 tabs, 2 figs

  15. Hierarchical CaCO3 chromatography: a stationary phase based on biominerals.

    Science.gov (United States)

    Sato, Kosuke; Oaki, Yuya; Takahashi, Daisuke; Toshima, Kazunobu; Imai, Hiroaki

    2015-03-23

    In biomineralization, acidic macromolecules play important roles for the growth control of crystals through a specific interaction. Inspired by this interaction, we report on an application of the hierarchical structures in CaCO3 biominerals to a stationary phase of chromatography. The separation and purification of acidic small organic molecules are achieved by thin-layer chromatography and flash chromatography using the powder of biominerals as the stationary phase. The unit nanocrystals and their oriented assembly, the hierarchical structure, are suitable for the adsorption site of the target organic molecules and the flow path of the elution solvents, respectively. The separation mode is ascribed to the specific adsorption of the acidic molecules on the crystal face and the coordination of the functional groups to the calcium ions. The results imply that a new family of stationary phase of chromatography can be developed by the fine tuning of hierarchical structures in CaCO3 materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. High-performance thin-layer chromatographic methods in the evaluation of the antioxidant and anti-hyperglycemic activity of Myrmecodia platytyrea as a promising opportunity in diabetes treatment.

    Science.gov (United States)

    Agatonovic-Kustrin, S; Morton, D W; Adam, A; Mizaton, H H; Zakaria, H

    2017-12-29

    The steady increase of diabetes is becoming a major burden on health care systems. As diabetic complications arise from oxidative stress, an antioxidant therapy along with anti-diabetic drugs is recommended. Myrmecodia or ant plant is highly valued as a traditional medicine in West Papua. It is used as an alternative treatment for diabetes, as the substances produced by ants can reduce blood sugar levels. The aim of this study was to develop and establish high-performance thin-layer chromatographic (HPTLC)-bioautographic methods to measure the antioxidant and hypoglycemic effects in different extracts from Myrmecodia platytyrea and to compare them with sterol content. Antioxidant activity in methanol, ethanol, dichloromethane (DCM) and ethyl acetate (EA) extracts were measured with a direct HPTLC-2,2-diphenyl-1-picrylhydrazyl free radical (DPPH) assay, while hypoglycemic effects were assessed using a newly developed α-amylase inhibitory activity assay. Stigmasterol is observed, after derivatization with anisaldehyde, as purple colored zones under visible light at hRF values of 0.66. The highest antioxidant activity was observed in the ethanol extract which is rich in polyphenols and flavonoids, while the DCM extract did not show antioxidant activity, but had significant α-amylase inhibitory activity. The highest α-amylase inhibitory activity was observed in the EA and DCM extracts and was related to their stigmasterol content. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

  17. Comparative standardization study for determination of reserpine in Rauwolfia serpentina homoeopathic mother tinctures manufactured by different pharmaceutical industries using HPTLC as a check for quality control

    Directory of Open Access Journals (Sweden)

    Binit Kumar Dwivedi

    2017-01-01

    Full Text Available Background: Rauwolfia serpentina (L. Benth. ex Kurz (Apocynaceae (Indian snakeroot, popularly known as Sarpagandha (Sanskrit, is used for the treatment of insanity, fever, snake bites, anxiety and in neuropsychiatric conditions. The antihypertensive actions of Reserpine are a result of its ability to deplete catecholamines (amongst other monoamine neurotransmitters from peripheral sympathetic nerve endings which are normally involved in controlling heart rate, force of cardiac contraction and peripheral vascular resistance. Objective: Comparative study of Reserpine content in R. serpentina homoeopathic mother tinctures manufactured by different pharmaceutical industries and in-house mother tinctures applying high-performance thin-layer chromatography investigative techniques to facilitate the use of correct species. Materials and Methods: The authentic samples of roots of R. serpentina were supplied by Centre of Medicinal Plants Research in Homoeopathy, Emerald, Tamil Nadu, India. Authentic plant material was used to prepare the mother tincture (as per Homoeopathic Pharmacopoeia of India. Reserpine (C33H40N2O9,M.P. 360°C, purity >99% w/w by high-performance liquid chromatography [HPLC] was purchased from Sigma-Aldrich as a standard reference. The solvents for the study, namely, ethanol, HPLC water, toluene, ethyl acetate, diethylamine and chloroform were of analytical grade purity (MERCK Ltd.,, used throughout. Results: Five samples of mother tinctures were used for the study, in-house mother tinctures (labelled: D and E of R. serpentina shows a higher amount of Reserpine content than the marketed samples (labelled: A, B and C. Conclusion: It may be concluded that mother tinctures prepared by authentic plants showed the excess amount of Reserpine rather than that of mother tinctures procured from the market.

  18. Attenuating effect of standardized lyophilized Cinnamomum zeylanicum bark extract against streptozotocin-induced experimental dementia of Alzheimer's type.

    Science.gov (United States)

    Malik, Jai; Munjal, Kavita; Deshmukh, Rahul

    2015-05-01

    The Cinnamomum zeylanicum (CZ; family Lauraceae) bark, an important spice, has also been used traditionally for nervous stress, as a nervine tonic, and as a stimulant. Therefore, the present study was designed to evaluate the effect of the standardized lyophilized aqueous extract of CZ bark (LCZE) on learning and memory in rodents at 50, 100, and 200 mg/kg, p.o. dose levels against streptozotocin (STZ)-induced memory impairment. LCZE was standardized based on the cinnamaldehyde content using high-performance thin-layer chromatography (HPTLC). The effect on learning and memory was evaluated using two widely used behavioral models, the Morris water maze (MWM) test and the object recognition test (ORT). The effect of LCZE on the acetylcholinesterase (AChE) activity and oxidative stress parameters in the cerebral cortex and hippocampus of rat brain was also evaluated. LCZE significantly (p<0.05) and dose-dependently attenuated STZ-induced cognitive deficit in both models in comparison to only STZ-treated animals. In the MWM test, LCZE (100 and 200 mg/kg) significantly decreased the transfer latency and increased the time spent by the animals in target quadrant. Similarly in the ORT, the LCZE-treated animals exhibited an improved discrimination between a familiar object and a novel object, indicating the reversal of STZ-induced memory impairment. LCZE also restored STZ-induced alteration in AChE activity and oxidative stress parameters in both brain parts. The results clearly indicate toward the memory-enhancing effect of LCZE, which could be due to the synergistic effect of anti-AChE and antioxidant activities.

  19. A new application of micellar liquid chromatography in the determination of free ampicillin concentration in the drug-human serum albumin standard solution in comparison with the adsorption method.

    Science.gov (United States)

    Stępnik, Katarzyna E; Malinowska, Irena; Maciejewska, Małgorzata

    2016-06-01

    The determination of free drug concentration is a very important issue in the field of pharmacology because only the unbound drug fraction can achieve a pharmacological effect. Due to the ability to solubilize many different compounds in micellar aggregates, micellar liquid chromatography (MLC) can be used for direct determination of free drug concentration. Proteins are not retained on the stationary phase probably due to the formation of protein - surfactant complexes which are excluded from the pores of stationary phase. The micellar method is simple and fast. It does not require any pre-preparation of the tested samples for analysis. The main aim of this paper is to demonstrate a completely new applicability of the analytical use of MLC concerning the determination of free drug concentration in the standard solution of human serum albumin. The well-known adsorption method using RP-HPLC and the spectrophotometric technique was applied as the reference method. The results show that the free drug concentration value obtained in the MLC system (based on the RP-8 stationary phase and CTAB) is similar to that obtained by the adsorption method: both RP-HPLC (95.83μgmL(-1), 79.86% of free form) and spectrophotometry (95.71μgmL(-1), 79.76%). In the MLC the free drug concentration was 93.98μgmL(-1) (78.3%). This indicates that the obtained results are within the analytical range of % of free ampicillin fraction and the MLC with direct sample injection can be treated like a promising method for the determination of free drug concentration. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Determination of high-molecular weight polycyclic aromatic hydrocarbons in high performance liquid chromatography fractions of coal tar standard reference material 1597a via solid-phase nanoextraction and laser-excited time-resolved Shpol'skii spectroscopy.

    Science.gov (United States)

    Wilson, Walter B; Alfarhani, Bassam; Moore, Anthony F T; Bisson, Cristina; Wise, Stephen A; Campiglia, Andres D

    2016-02-01

    This article presents an alternative approach for the analysis of high molecular weight - polycyclic aromatic hydrocarbons (HMW-PAHs) with molecular mass 302 Da in complex environmental samples. This is not a trivial task due to the large number of molecular mass 302 Da isomers with very similar chromatographic elution times and similar, possibly even virtually identical, mass fragmentation patterns. The method presented here is based on 4.2K laser-excited time-resolved Shpol'skii spectroscopy, a high resolution spectroscopic technique with the appropriate selectivity for the unambiguous determination of PAHs with the same molecular mass. The potential of this approach is demonstrated here with the analysis of a coal tar standard reference material (SRM) 1597a. Liquid chromatography fractions were submitted to the spectroscopic analysis of five targeted isomers, namely dibenzo[a,l]pyrene, dibenzo[a,e]pyrene, dibenzo[a,i]pyrene, naphtho[2,3-a]pyrene and dibenzo[a,h]pyrene. Prior to analyte determination, the liquid chromatographic fractions were pre-concentrated with gold nanoparticles. Complete analysis was possible with microliters of chromatographic fractions and organic solvents. The limits of detection varied from 0.05 (dibenzo[a,l]pyrene) to 0.24 µg L(-1) (dibenzo[a,e]pyrene). The excellent analytical figures of merit associated to its non-destructive nature, which provides ample opportunity for further analysis with other instrumental methods, makes this approach an attractive alternative for the determination of PAH isomers in complex environmental samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Delamination of Compressed Thin Layers at Corners

    DEFF Research Database (Denmark)

    Sørensen, Kim D.; Jensen, Henrik Myhre; Clausen, Johan

    2008-01-01

    An analysis of delamination for a thin elastic layer under compression, attached to a substrate at a corner is carried out. The analysis is performed by combining results from interface fracture mechanics and the theory of thin shells. In contrast with earlier results for delamination on a flat...... results for the fracture mechanical properties have been obtained, and these are applied in a study of the effect of contacting crack faces. Special attention has been given to analyse conditions under which steady state propagation of buckling driven delamination takes place. Keywords: Delamination, Thin...

  2. Recent advances in thin-layer cytology.

    Science.gov (United States)

    Linder, J

    1998-01-01

    In recent years liquid-based cytology has emerged as an alternative to conventional cytopreparatory methods. In particular, the ThinPrep system has found broad acceptance in non-gynecologic cytopreparation. Many laboratories have successfully applied this technique to body fluids (e.g. urine, pleural effusions), brushing samples (e.g. gastrointestinal tract, lung) and fine-needle aspiration. Most comparative studies have shown the ThinPrep system to perform as well as or better than conventional preparations in nongynecologic cytology; plus, the residual cells within the vial can be used for DNA analysis or immunohistochemical and other special studies. Recently, the ThinPrep 2000 system has been approved for use in gynecologic cytology. This approval was based on a large, multicenter clinical study that showed the ThinPrep system to be favored over the conventional Pap smear for the detection of low-grade squamous intraepithelial lesions, or more severe lesions. At screening centers the improved rate of detecting low grade squamous intraepithelial lesions (LSIL) or more severe diagnosis was up to 73%, with an average improvement of 65% as compared to the conventional Pap smears. Also, for specimen adequacy, the ThinPrep method was statistically favored over conventional cytology methods. This multicenter clinical trial demonstrates the ThinPrep 2000 system was more effective than the conventional Pap smear for the detection of atypical cells and cervical cancer and its precursor lesions. In addition, by collecting cells in a liquid-based medium the opportunity is present to improve the Pap test by adjunctive testing for Human Papilloma Virus or other procedures. This creates the opportunity for improved triage and management of patients with cervical abnormalities.

  3. Thin layer Characterization by ZGV Lamb modes

    Science.gov (United States)

    Cès, Maximin; Clorennec, Dominique; Royer, Daniel; Prada, Claire

    2011-01-01

    Ultrasonic non-destructive testing of plates can be performed with Lamb modes guided by the structure. Non contact generation and detection of the elastic waves can be achieved with optical means such as a pulsed laser source and an interferometer. With this setup, we propose a method using zero group velocity (ZGV) Lamb modes rather than propagating modes. These ZGV modes have noteworthy properties, in particular their group velocity vanishes, whereas their phase velocity remains finite. Thus, a significant part of the energy deposited by the pulsed laser can be trapped in the source area. For example, in a homogeneous isotropic plate and at the minimum frequency of the S1-Lamb mode a very sharp resonance can be observed, the frequency of which only depends on the plate thickness, for a given material. In fact, other ZGV modes exist and the set of ZGV resonance frequencies provide a local and absolute measurement of Poisson's ratio. These non-propagating modes can also be used to characterize multi-layered structures. Experimentally, we observed that a thin (500 nm) gold layer deposited on a thick (1.5 mm) Duralumin plate induces a sensitive down-shift of the set of ZGV resonance frequencies. This shift, which is typically 5 kHz for the S1-Lamb mode at 1.924 MHz, can be approximated by a formula providing the layer thickness. Thickness down to 100 nm can be estimated by this method. Such a sensitivity with conventional ultrasound inspection by acoustic microscopy would require an operating frequency in the GHz range.

  4. Defect free single crystal thin layer

    KAUST Repository

    Elafandy, Rami Tarek Mahmoud

    2016-01-28

    A gallium nitride film can be a dislocation free single crystal, which can be prepared by irradiating a surface of a substrate and contacting the surface with an etching solution that can selectively etch at dislocations.

  5. EXPERIMENTAL FORCED SOLAR THIN LAYER GINGER DRYING

    Directory of Open Access Journals (Sweden)

    Mahesh Kumar

    2016-04-01

    Full Text Available In this research paper, the convective and the evaporative heat transfer coefficients of ginger (zingiber officinale drying in an indirect solar cabinet dryer under the induced forced convection mode is presented. Experiments were conducted during the month of March 2015 under the climatic conditions of Hisar, India (29°5’5”N latitude and 75°45’55”E longitude. The experimental data obtained for solar drying of a constant ginger mass of 150 g has been used to determine constants ‘C’ and ‘n’ in the Nusselt number expression using linear regression analysis; consequently, the convective and the evaporative heat transfer coefficients have been evaluated. The average value of constants ‘C’ and ‘n’ were evaluated as 0.999 and 0.318, respectively. The average values of the convective and the evaporative heat transfer coefficients were found to be 3.95 W/m2 °C and 160.47 W/m2 °C, respectively, for the given mass samples of ginger. The average collector efficiency was observed to be 14.5%. The experimental error in terms of percentage uncertainty was found to be 20.87%.

  6. Delamination of Compressed thin Layers at Corners

    DEFF Research Database (Denmark)

    Clausen, Johan; Jensen, Henrik Myhre; Sørensen, Kim Dalsten

    2008-01-01

    An analysis of delamination for a thin elastic film, attached to a substrate with a corner, is carried out. The film is in compression and the analysis is performed by combining results from fracture mechanics and the theory of thin shells. The results show a very strong dependency of the angle...

  7. Delamination of Compressed Thin Layers at Corners

    DEFF Research Database (Denmark)

    Sørensen, Kim Dalsten; Jensen, Henrik Myhre; Clausen, Johan

    2008-01-01

    An analysis of delamination for a thin elastic layer under compression, attached to a substrate at a corner is carried out. The analysis is performed by combining results from interface fracture mechanics and the theory of thin shells. In contrast with earlier results for delamination on a flat...

  8. Identification of reaction products of methamphetamine and hydrogen peroxide in hair dye and decolorant treatments by high-performance liquid chromatography/mass spectrometry.

    Science.gov (United States)

    Tanaka, S; Iio, R; Chinaka, S; Takayama, N; Hayakawa, K

    2001-02-01

    The effect of hydrogen peroxide, a main component of hair dye and decolorant treatments, on methamphetamine (MA) was studied. Two analytical methods, thin-layer chromatography (TLC) and high-performance liquid chromatography/mass spectrometry (LC/MS), were used for the separation and identification of MA derivatives. Mixtures of MA solutions and hydrogen peroxide that had been incubated at 39 degrees C for 24 h were shown to contain para-hydroxy MA by TLC and para-, meta- and ortho-hydroxy MAs by LC/MS. In addition, MA N-oxide and N-hydroxy MA were found in MA/hydrogen peroxide mixtures immediately after mixing. Therefore, we concluded that MA changed to MA N-oxide and N-hydroxy MA before changing to para-, meta- and ortho-hydroxy MAs.

  9. Chromatography resin support

    Science.gov (United States)

    Dobos, James G.

    2002-01-01

    An apparatus and method of using an improved chromatography resin support is disclosed. The chromatography support platform is provided by a stainless steel hollow cylinder adapted for being inserted into a chromatography column. An exterior wall of the stainless steel cylinder defines a groove for carrying therein an "O"-ring. The upper surface of the stainless steel column is covered by a fine stainless steel mesh welded to the edges of the stainless steel cylinder. When placed upon a receiving ledge defined within a chromatography column, the "O"-ring provides a fluid tight seal with the inner edge wall of the chromatography cylinder. The stainless steel mesh supports the chromatography matrix and provides a back flushable support which is economical and simple to construct.

  10. Application of modified hollow fiber liquid phase microextraction in conjunction with chromatography-electron capture detection for quantification of acrylamide in waste water samples at ultra-trace levels.

    Science.gov (United States)

    Sobhi, Hamid Reza; Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali

    2017-03-03

    Herein, a simple and sensitive method was successfully developed for the extraction and quantification of acrylamide in water samples. Initially, acrylamide was derivatized through a bromination process. Subsequently, a modified hollow-fiber liquid-phase microextraction was applied for the extraction of the brominated acrylamide from a 10-ml portion of an aqueous sample. Briefly, in this method, the derivatized acrylamide (2,3-dibromopropionamide) was extracted from the aqueous sample into a thin layer of an organic solvent sustained in pores of a porous hollow fiber. Then, it was back-extracted using a small volume of organic acceptor solution (acetonitril, 25μl) located inside the lumen of the hollow fiber followed by gas chromatography-electron capture detection (GC-ECD). The optimal conditions were examined for the extraction of the analyte such as: the organic solvent: dihexyl ether+10% tri-n-octyl phosphine oxide; stirring rate: 750rpm; no salt addition and 30min extraction time. These optimal extraction conditions allowed excellent enrichment factor values for the method. Enrichment factor, detection limit (S/N=3) and dynamic linear range of 60, 2ngL-1 and 50-1000ngL-1 to be determined for the analyte. The relative standard deviations (RSD%) representing precision of the method were in the range of 2.2-5.8 based on the average of three measurements. Accuracy of the method was tested by the relative recovery experiments on spiked samples, with results ranging from 93 to 108%. Finally, the method proved to be simple, rapid, and cost-effective for routine screen of acrylamide-contaminated highly-complicated untreated waste water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Facile preparation of polyvinyl alcohol coated SiO2 stationary phases for high performance liquid chromatography.

    Science.gov (United States)

    Ji, Shunli; Zhang, Feifang; Wu, Shengjie; Yang, Bingcheng; Liang, Xinmiao

    2014-11-07

    A facile method to prepare a polar stationary phase for hydrophilic interaction chromatography (HILIC) was proposed by coating polyvinyl alcohol onto silica particles (PVA-Sil). A water or organic solvent-insoluble permanent PVA coating on the silica particle surface can be formed simply by dipping silica particles into a hot PVA solution and then settled from this solution, leaving a thin layer of PVA coating and frozen in a freezer. The PVA-Sil shields the silica core from solution erosion to some degree and the pH tolerance range was extended to 9.5 from 8.0 for bare silica. PVA-Sil demonstrated a good hydrophilic property for several kinds of polar compounds and ∼57000 m(-1) of plate count was achieved. This method can also be extended as a universal method to prepare various stationary phases with exchangeable functionalities by doping the desired ingredient in a PVA solution.

  12. [Identification of 4-O-methyldopamine in rat tissues by reverded-phase liquid chromatography (author's transl)].

    Science.gov (United States)

    Bidard, J N; Cronenberger, L

    1979-10-11

    4-O-Methyldopamine was identified and assayed in tissues from L-dopa treated rats by reversed-phase high-performance liquid chromatography. The initial steps in the separation of catecholamines were performed by alumine, a weak cation-exchange resin, and thin-layer chromatographic techniques. After L-[3 H] dopa administration, the radiochromatogram was superimposed on the fluorochromatogram obtained with authentic marker 4-O-methyldopamine. This metabolite was detected in kidney but not in brain. The 4-O-methyldopamine:3-O-methyldopamine ratio was 0.032 in kidney. The influence of various treatments on this ratio was investigated. A 160% increase was found after L-dopa administration. This effect was potentiated by nialamide pretreatment (550% increase).

  13. Laboratory and field based evaluation of chromatography ...

    Science.gov (United States)

    The Monitor for AeRosols and GAses in ambient air (MARGA) is an on-line ion-chromatography-based instrument designed for speciation of the inorganic gas and aerosol ammonium-nitrate-sulfate system. Previous work to characterize the performance of the MARGA has been primarily based on field comparison to other measurement methods to evaluate accuracy. While such studies are useful, the underlying reasons for disagreement among methods are not always clear. This study examines aspects of MARGA accuracy and precision specifically related to automated chromatography analysis. Using laboratory standards, analytical accuracy, precision, and method detection limits derived from the MARGA chromatography software are compared to an alternative software package (Chromeleon, Thermo Scientific Dionex). Field measurements are used to further evaluate instrument performance, including the MARGA’s use of an internal LiBr standard to control accuracy. Using gas/aerosol ratios and aerosol neutralization state as a case study, the impact of chromatography on measurement error is assessed. The new generation of on-line chromatography-based gas and particle measurement systems have many advantages, including simultaneous analysis of multiple pollutants. The Monitor for Aerosols and Gases in Ambient Air (MARGA) is such an instrument that is used in North America, Europe, and Asia for atmospheric process studies as well as routine monitoring. While the instrument has been evaluat

  14. Comparative study of three Marantodes pumilum varieties by microscopy, spectroscopy and chromatography

    Directory of Open Access Journals (Sweden)

    Nor-Ashila Aladdin

    Full Text Available Abstract Marantodes pumilum (Blume Kuntze (synonym: Labisia pumila (Blume Fern.-Vill, Primulaceae, is well known for its traditional use as a post-partum medication among women in Malaysia. Three varieties of M. pumilum, var. alata Scheff., var. pumila and var. lanceolata (Scheff. Mez. are commonly used. Nowadays, M. pumilum powder or extracts are commercially available as herbal supplements and beverages. Authentication of the variety is an important component of product quality control. Thus, the present work was aimed to compare the three varieties using microscopic, spectroscopic and chromatographic techniques. Microscopic anatomical examination and powder microscopy were performed on fresh and dried plant materials, respectively. Fingerprint profiles of the varieties were obtained using attenuated total reflectance-Fourier transform infrared spectrophotometer, high performance thin layer chromatography and high performance liquid chromatography. The microscopic examination showed presence of anisocytic stomata, scale and capitate glandular trichome in all varieties. The type of stomata and trichomes, outline structure of stem and leaf margin, petiole and midrib, organization of vascular system, areolar venation, pattern of anticlinal walls, the distribution of secretory canals and cell inclusion as well as the measurement of selected structures could be used to distinguish and identify each variety of M. pumilum. In addition, spectroscopic and chromatographic fingerprint analyses of the three varieties exhibited distinguishable profiles based on the intensity of certain peaks or bands. The findings from this study will provide systematic identification for these varieties.

  15. Chemistry and liquid chromatography methods for the analyses of primary oxidation products of triacylglycerols.

    Science.gov (United States)

    Zeb, A

    2015-05-01

    Triacylglycerols (TAGs) are one of the major components of the cells in higher biological systems, which can act as an energy reservoir in the living cells. The unsaturated fatty acid moiety is the key site of oxidation and formation of oxidation compounds. The TAG free radical generates several primary oxidation compounds. These include hydroperoxides, hydroxides, epidioxides, hydroperoxy epidioxides, hydroxyl epidioxides, and epoxides. The presence of these oxidized TAGs in the cell increases the chances of several detrimental processes. For this purpose, several liquid chromatography (LC) methods were reported in their analyses. This review is therefore focused on the chemistry, oxidation, extraction, and the LC methods reported in the analyses of oxidized TAGs. The studies on thin-layer chromatography were mostly focused on the total oxidized TAGs separation and employ hexane as major solvent. High-performance LC (HPLC) methods were discussed in details along with their merits and demerits. It was found that most of the HPLC methods employed isocratic elution with methanol and acetonitrile as major solvents with an ultraviolet detector. The coupling of HPLC with mass spectrometry (MS) highly increases the efficiency of analysis as well as enables reliable structural elucidation. The use of MS was found to be helpful in studying the oxidation chemistry of TAGs and needs to be extended to the complex biological systems.

  16. Particle size effects on protein and virus-like particle adsorption on perfusion chromatography media.

    Science.gov (United States)

    Wu, Yige; Abraham, Dicky; Carta, Giorgio

    2015-01-02

    The resin structure, chromatographic behavior, and adsorption kinetics of proteins and virus-like-particles (VLPs) are studied for POROS HS 20 and POROS HS 50 (23 and 52 μm mean diameter, respectively) to determine the effects of particle size on perfusion chromatography and to determine the predictive ability of available models. Transmission electron microscopy (TEM) and inverse size-exclusion chromatography (iSEC) show similar structures for the two resins, both containing 200-1000 nm pores that transect a network of much smaller pores. For non-binding conditions, trends of the height equivalent to a theoretical plate (HETP) as a function of reduced velocity are consistent with perfusion. The estimated intraparticle flow fractions for these conditions are 0.0018 and 0.00063 for POROS HS 20 and HS 50, respectively. For strong binding conditions, confocal laser scanning microscopy (CLSM) shows asymmetrical intraparticle concentrations profiles and enhanced rates of IgG adsorption on POROS HS 20 at 1000 cm/h. The corresponding effective diffusivity under flow is 2-3 times larger than for non-flow conditions and much larger than observed for POROS HS 50, consistent with available models. For VLPs, however, adsorption is confined to a thin layer near the particle surface for both resins, suggesting that the bound VLPs block the pores. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. [Frontal displacement chromatography of melittin on meshed polymer ionites].

    Science.gov (United States)

    Pisarev, O A; Iunysheva, S G; Samsonov, G V

    1998-01-01

    Conditions of frontal displacement chromatography were optimized for preparative purification of the polypeptide hormone melittin from bee venom. Melittin was purified to an extent higher than that of a standard preparation described in the biochemical literature.

  18. High Performance Liquid Chromatography

    Science.gov (United States)

    Talcott, Stephen

    High performance liquid chromatography (HPLC) has many applications in food chemistry. Food components that have been analyzed with HPLC include organic acids, vitamins, amino acids, sugars, nitrosamines, certain pesticides, metabolites, fatty acids, aflatoxins, pigments, and certain food additives. Unlike gas chromatography, it is not necessary for the compound being analyzed to be volatile. It is necessary, however, for the compounds to have some solubility in the mobile phase. It is important that the solubilized samples for injection be free from all particulate matter, so centrifugation and filtration are common procedures. Also, solid-phase extraction is used commonly in sample preparation to remove interfering compounds from the sample matrix prior to HPLC analysis.

  19. Clinical applications of gas chromatography and gas chromatography-mass spectrometry of steroids

    NARCIS (Netherlands)

    Wolthers, BG; Kraan, GPB

    1999-01-01

    This review article underlines the importance of gas chromatography-mass spectrometry (GC-MS) for determination of steroids in man. The use of steroids labelled with stable isotopes as internal standard and subsequent analysis by GC-MS yields up to now the only reliable measurement of steroids in

  20. Fully automated determination of the sterol composition and total content in edible oils and fats by online liquid chromatography-gas chromatography-flame ionization detection.

    Science.gov (United States)

    Nestola, Marco; Schmidt, Torsten C

    2016-09-09

    Sterol analysis of edible oils and fats is important in authenticity control. The gas chromatographic determination of the sterol distribution and total content is described by ISO norm 12228. Extraction, purification, and detection of the sterols are time-consuming and error-prone. Collaborative trials prove this regularly. Purification by thin-layer chromatography (TLC) and robust GC determination of all mentioned sterols is not straightforward. Therefore, a fully automated LC-GC-FID method was developed to facilitate the determination of sterols. The only manual step left was to weigh the sample into an autosampler vial. Saponification and extraction were performed by an autosampler while purification, separation, and detection were accomplished by online coupled normal-phase LC-GC-FID. Interlacing of sample preparation and analysis allowed an average sample throughput of one sample per hour. The obtained quantitative results were fully comparable with the ISO method with one apparent exception. In the case of sunflower oils, an additional unknown sterol was detected generally missed by ISO 12228. The reason was found in the omission of sterol silylation before subjection to GC-FID. The derivatization reaction changed the retention time and hid this compound behind a major sterol. The compound could be identified as 14-methyl fecosterol. Its structure was elucidated by GC-MS and ensured by HPLC and GC retention times. Finally, validation of the designed method confirmed its suitability for routine environments. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Wound Healing Activity and Chemical Standardization of Eugenia pruniformis Cambess.

    Science.gov (United States)

    de Albuquerque, Ricardo Diego Duarte Galhardo; Perini, Jamila Alessandra; Machado, Daniel Escorsim; Angeli-Gamba, Thaís; Esteves, Ricardo Dos Santos; Santos, Marcelo Guerra; Oliveira, Adriana Passos; Rocha, Leandro

    2016-01-01

    . The total flavonoid content was 43% (w/w) and quercetin, kaempferol and hyperoside were identified as main compounds. Wound excision model in rats showed the potential wound healing activity of E. pruniformis by collagen deposition increase, higher levels of hidroxyproline, better tissue reorganization and complete remodeling of epidermis.Flavonoids are the main compounds of the endemic E. pruniformis and quercetin, kaempferol and hyperoside were identified in ethyl acetate extract by TLC, HPLC-PDA and HRESI-MS analysis.The ethyl acetate extract of E. pruniformis showed a potent antioxidant activity by ORAC and DPPH assays Abbreviation used: NC: Negative control, PC: Positive control, CH: Crude hydroethanolic extract, EA: Ethyl acetate extract, TE: Trolox equivalent, mg: Milligram, mM: Millimolar, mL: Milliliter, HPLC-PDA: High performance liquid chromatography with a photodiode array detector, HRESI-MS: High-resolution electrospray ionization mass spectrometry analysis, TLC: Thin layer chromatography, ORAC: Oxygen radical absorbance capacity, w/v: Weight per volume.

  2. Size fractionation by slalom chromatography and hydrodynamic chromatography

    OpenAIRE

    Dias, Ricardo P.

    2008-01-01

    Hydrodynamic chromatography, also called separation by flow, is based on the use of the parabolic flow profile occurring in open capillaries or in the pores from a column filled with non-porous particles. The hydrodynamic chromatography separation medium, if any, is much simpler than that from size exclusion chromatography (porous particles), the former technique being used in the size-fractionation of many colloids and macromolecules. The transition between hydrodynamic chromatography (obtai...

  3. performance liquid chromatography

    African Journals Online (AJOL)

    user

    2010-11-22

    Nov 22, 2010 ... This study is aimed to determine the concentration of acrylamide in processed food products available in open market. In order to determine the acrylamide concentration, three bakery items and three fried chips from three different brands were analyzed. High-performance liquid chromatography (HPLC) ...

  4. Optimized Formation of Benzyl Isothiocyanate by Endogenous ...

    African Journals Online (AJOL)

    The formed benzyl isothiocyanate was extracted by steam distillation method and purified by thin-layer chromatography (TLC). Relevant process variables were also studied. Finally, the purified benzyl isothiocyanate was analyzed by gas chromatography-mass spectrometer (GC-MS) and compared to BITC standard.

  5. Quality Control of Tanzanian Curcuma longa L. Rhizome: An Anti ...

    African Journals Online (AJOL)

    Powdered plant material were then extracted in methanol and the extract used for carrying out other identity tests including thin layer chromatography and high performance liquid chromatography, curcumin as a standard. Quality tests like total ash, acid insoluble, water and alcohol soluble extractives, curcumin and volatile ...

  6. Improved Thermal Modulator for Gas Chromatography

    Science.gov (United States)

    Hasselbrink, Ernest Frederick, Jr.; Hunt, Patrick J.; Sacks, Richard D.

    2008-01-01

    An improved thermal modulator has been invented for use in a variant of gas chromatography (GC). The variant in question denoted as two-dimensional gas chromatography (2DGC) or GC-GC involves the use of three series-connected chromatographic columns, in the form of capillary tubes coated interiorly with suitable stationary phases (compounds for which different analytes exhibit different degrees of affinity). The two end columns are relatively long and are used as standard GC columns. The thermal modulator includes the middle column, which is relatively short and is not used as a standard GC column: instead, its temperature is modulated to affect timed adsorption and desorption of analyte gases between the two end columns in accordance with a 2DGC protocol.

  7. [Chromatographic identification and analysis of dextromoramide in the plasma by the method of high performance liquid chromatography].

    Science.gov (United States)

    Misztal, G; Przyborowski, L; Jednacz, T

    1989-01-01

    Dextromoramide and pethidine were separated and identified by thin-layer chromatography on silica gel, using ammonia and methanol (1.5:100) as the mobile phase, after previous extraction with dicthyl ether or with a mixture of n-hexane and isoamyl alcohol (98.5:1.5) from blood alkalized to pH 10.3 Dextromoramide can be revealed on the chromatograms in the amount of 0.5 micrograms and pethidine in the amount of 1 micrograms using the Dragendorff reagent. Reversed-phase TLC proved less sensitive. High-performance liquid chromatography on the column of LiChrosorb RP-18 was applied to the determination of dextromoramide in blood after extraction with diethyl ether, using methanol--phosphate buffer pH 4.5 (95:5) as the mobile phase. The determination range was of 0.5-5.0 micrograms per 2 cm3 of blood plasma (1.26.10(-8)-1.26.10(-7) mole/dm3).

  8. Physicochemical standardization, HPTLC profiling, and biological evaluation of Aśvagandhādyariṣṭa: A comparative study of three famous commercial brands

    Science.gov (United States)

    Singh, Mandeep; Kaur, Navdeep; Paul, Atish Tulsiram

    2014-01-01

    Background: Aśvagandhādyariṣṭa is a polyherbal formulation that is available commercially as an over the counter drug. There are three famous brands that are available in the market. However, there are no comparative reports on the physicochemical, chromatographic, and biological profiles of Aśvagandhādyariṣṭa manufactured by these famous companies. Aims: The present study deals with the physicochemical standardization, high performance thin layer chromatography (HPTLC) profiling, and biological evaluation of Aśvagandhādyariṣṭa. Materials and Methods: Aśvagandhādyariṣṭa manufactured by three leading companies were purchased from Jalandhar, Punjab. The physicochemical standardization of the samples was carried out in accordance with the Ayurvedic Pharmacopoeia of India (API). Authentified Eisenia foetida were procured from Ujjwal Ujala Vermiculture Group, Amritsar. The anthelmintic activity, 1,1-diphenyl-2-picrylhydrazyl scavenging, and hydrogen peroxide scavenging ability of Aśvagandhādyariṣṭa was determined. Statistical Analysis Used: The data of anthelmintic activity were expressed as mean ± standard error of the mean of six earthworms in each group. The statistical analysis was carried out using one-way analysis of variance, followed by Dunnet t-test. The difference in values at P .05 was considered to be statistically significant. Results: Most of the physicochemical standardization parameters mentioned as per the API were found to be within limit. HPTLC profiling showed the presence of withanolide D in commercial samples. Out of three commercial brands, ASA-DAB was the most active as compared to the ASA-BDN and ASA-AVP at the concentration of 200 mg/ml for anthelmintic activity against E. foetida. ASA-DAB showed the best antioxidant activity in both the in vitro assay at the concentration of 100 μg/ml. Conclusions: The ability of this formulation to scavenge free radicals supports its medical claim of antistress formulation. The

  9. Evaluation and prevention of the negative matrix effect of terpenoids on pesticides in apples quantification by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie

    2017-02-03

    The sample matrix can enhance the gas chromatography signal of pesticide residues relative to that obtained with the same concentration of pesticide in solvent. This paper is related to negative matrix effects observed in coupled gas chromatography-mass spectrometry ion trap (GC/MS2) quantification of pesticides in concentrated extracts of apple peel prepared by the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) method. It is focused on the pesticides most frequently used on the apple varieties studied, throughout the crop cycle, right up to harvest, to combat pests and diseases and to improve fruit storage properties. Extracts from the fleshy receptacle (flesh), the epiderm (peel) and fruit of three apple varieties were studied by high-performance thin-layer chromatography hyphenated with UV-vis light detection (HPTLC/UV visible). The peel extracts had high concentrations of triterpenic acids (oleanolic and ursolic acids), reaching 25mgkg-1, whereas these compounds were not detected in the flesh extracts (matrix effects in GC/MS2. The differences in the behavior of pesticides with respect to matrix effects can be accounted for by the physicochemical characteristics of the molecules (lone pairs, labile hydrogen, conjugation). The HPTLC/UV visible method developed here for the characterization of QuEChERS extracts acts as a complementary clean-up method, aimed to decrease the negative matrix effects of such extracts. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Detection of flavonoids in Alpinia purpurata (Vieill. K. Schum. leaves using high-performance liquid chromatography Detecção de flavonóides em folhas de Alpinia purpurata (Vieill. K. Schum. por cromatografia líquida de alta eficiência

    Directory of Open Access Journals (Sweden)

    C.P. Victório

    2009-01-01

    Full Text Available The species Alpinia purpurata is scarcely cited as to ethnopharmacology and phytochemistry. This study aimed to analyze bioactive compounds through high-performance liquid chromatography (HPLC. Hydroalcoholic crude extract was obtained from A. purpurata dried leaves. Folin-Ciocalteau method was used to quantify total phenols, using gallic acid as standard. The obtained result was 15.6 mg GAE g-1. The crude extract was partitioned with the solvents ethyl acetate and butanol, followed by thin-layer chromatography (TLC and HPLC. The flavonoids kaempferol-3-O-glucuronide and rutin were detected at a higher concentration in ethyl acetate and butanolic extracts. The butanolic extract contains the highest flavonoid percentage (94.3%. A. purpurata presents important flavonoids of therapeutic use, already verified for A. zerumbet. This is the first study verifying the presence of flavonoids in A. purpurata extracts.A espécie Alpinia purpurata apresenta poucas citações referentes a etnofarmacologia e fitoquímica. Este estudo propõe a análise de substâncias bioativas através da técnica de cromatografia líquida de alta eficiência (CLAE. O extrato bruto hidroalcóolico foi obtido a partir de folhas secas de A. purpurata. A quantificação de fenóis totais foi realizada pelo método de Folin-Ciocalteau, usando ácido gálico como padrão. Como resultado, foi verificado 15,6 mg EAG g-1. O extrato bruto foi particionado com os solventes acetato de etila e butanol e depois analisado por cromatografia em camada delgada e CLAE. Nos extratos acetato de etila e butanólico foi detectada a presença dos flavonóides kaempferol-3-O-glicuronídeo e rutina, em maior concentração. O extrato butanólico contém a maior porcentagem de flavonóides (94,3%. Esta espécie possui flavonóides importantes no uso terapêutico, já antes verificados para a espécie A. zerumbet. Este é o primeiro trabalho que verifica a presença de flavonóides em extratos de A

  11. Spiral Countercurrent Chromatography

    Science.gov (United States)

    Ito, Yoichiro; Knight, Martha; Finn, Thomas M.

    2013-01-01

    For many years, high-speed countercurrent chromatography conducted in open tubing coils has been widely used for the separation of natural and synthetic compounds. In this method, the retention of the stationary phase is solely provided by the Archimedean screw effect by rotating the coiled column in the centrifugal force field. However, the system fails to retain enough of the stationary phase for polar solvent systems such as the aqueous–aqueous polymer phase systems. To address this problem, the geometry of the coiled channel was modified to a spiral configuration so that the system could utilize the radially acting centrifugal force. This successfully improved the retention of the stationary phase. Two different types of spiral columns were fabricated: the spiral disk assembly, made by stacking multiple plastic disks with single or four interwoven spiral channels connected in series, and the spiral tube assembly, made by inserting the tetrafluoroethylene tubing into a spiral frame (spiral tube support). The capabilities of these column assemblies were successfully demonstrated by separations of peptides and proteins with polar two-phase solvent systems whose stationary phases had not been well retained in the earlier multilayer coil separation column for high-speed countercurrent chromatography. PMID:23833207

  12. Evaluation of a Commercial Sandwich Enzyme-Linked Immunosorbent Assay for the Quantification of Beta-Casomorphin 7 in Yogurt Using Solid-Phase Extraction Coupled to Liquid Chromatography-Tandem Mass Spectrometry as the "Gold Standard" Method.

    Science.gov (United States)

    Nguyen, Duc Doan; Busetti, Francesco; Johnson, Stuart Keith; Solah, Vicky Ann

    2017-08-01

    This study investigated beta-casomorphin 7 (BCM7) in yogurt by means of LC-tandem MS (MS/MS) and enzyme-linkedimmunosorbent assay (ELISA) and use LC-MS/MS as the "gold standard" method to evaluate the applicability of a commercial ELISA. The level of BCM7 in milk obtained from ELISA analysis was much lower than that obtained by LC-MS/MS analysis and trended to increase during fermentation and storage of yogurt. Meanwhile, the results obtained from LC-MS/MS showed that BCM7 degraded during stages of yogurt processing, and its degradation may have been caused by X-prolyl dipeptidyl aminopeptidase activity. As a result, the commercial sandwich ELISA kit was not suitable for the quantification of BCM7 in fermented dairy milk.

  13. Ultra-Performance Liquid Chromatography Hyphenated with Quadrupole-Orbitrap Mass Spectrometry for Simultaneous Determination of Necine-Core-Structure Pyrrolizidine Alkaloids in Crotalaria sessiliflora L. without all Corresponding Standards.

    Science.gov (United States)

    Zhang, Wei; Huai, Wenbei; Zhang, Yi; Shen, Jincan; Tang, Xunyou; Xie, Xiujuan; Wang, Ke; Fan, Huajun

    2017-09-01

    Crotalaria sessiliflora L. is a Chinese traditional herb for treatment of cutaneum carcinoma and cervical carcinoma. In addition to monocrotaline, coexisting pyrrolizidine alkaloids (PAs) also require further quantification for quality control and pharmaceutical uses of the herb. To establish a UPLC-Q-Orbitrap/MS method of simultaneous determination of coexisting PAs with same parent structure for quality control and comprehensive researches of Crotalaria sessiliflora L. PAs in Crotalaria sessiliflora L. were analysed by UPLC-Q-Orbitrap/MS method. Coexisting PAs were identified by mass data of full MS-dd-MS2 based on the characteristic fragmentation pattern and necine-core structure. Moreover, quantification of PAs was conducted by parallel reaction monitoring (PRM) mode using m/z 138, m/z 120 and m/z 94 from identical necine-core structure as quantitative ions with single monocrotaline standard for accurate calibration. Five PAs, named monocrotaline, retrorsine, senecionine, integerrimine, O-9-angeloylretronecine, were indentified and confirmed. Quantitative ions of m/z 138, m/z 120 and m/z 94 were used for quantification of PAs containing the necine-core structure in Crotalaria sessiliflora L. The results demonstrated that contents, precision and recoveries of the five PAs mentioned earlier were respectively 3.307-30.35 μg/g, 1.1-4.5% and 88.91-92.33% while using m/z 120 as the best quantitative ion. The UPLC-Q-Orbitrap/MS method was established for simultaneous determination of five PAs in Crotalaria sessiliflora L. without all corresponding standards, and was proved that it was simple, convenient and effective for comprehensive quality control and pharmaceutical uses. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  14. Peak broadening in paper chromatography and related techniques

    NARCIS (Netherlands)

    Ligny, C.L. de; Veen, N.G. van

    1972-01-01

    Peak dispersion (i.e. the separation efficiency) in thin-layer electrophoresis was investigated and compared for six different cellulose layers. The relative importance of longitudinal diffusion and of macroscopic inhomoeneities in the electric field and in the electroosmotic and sucking flow

  15. Dielectrokinetic chromatography devices

    Science.gov (United States)

    Chirica, Gabriela S; Fiechtner, Gregory J; Singh, Anup K

    2014-12-16

    Disclosed herein are methods and devices for dielectrokinetic chromatography. As disclosed, the devices comprise microchannels having at least one perturber which produces a non-uniformity in a field spanning the width of the microchannel. The interaction of the field non-uniformity with a perturber produces a secondary flow which competes with a primary flow. By decreasing the size of the perturber the secondary flow becomes significant for particles/analytes in the nanometer-size range. Depending on the nature of a particle/analyte present in the fluid and its interaction with the primary flow and the secondary flow, the analyte may be retained or redirected. The composition of the primary flow can be varied to affect the magnitude of primary and/or secondary flows on the particles/analytes and thereby separate and concentrate it from other particles/analytes.

  16. Determination of multi-mycotoxins in cereals and of total fumonisins in maize products using isotope labeled internal standard and liquid chromatography/tandem mass spectrometry with positive ionization.

    Science.gov (United States)

    Andrade, Patrícia Diniz; Dantas, Rebecca Rodrigues; Moura-Alves, Tatiana Loureiro da Silva de; Caldas, Eloisa Dutra

    2017-03-24

    Mycotoxins are secondary fungi metabolites present in foods that cause adverse effects in humans and animals. The aims of this work were to develop and validate a multi-mycotoxin method to determine the presence of aflatoxins, citreoviridin, deoxynivalenol, fumonisins ochratoxin A, zearalenone and some metabolites/derivatives in rice, maize-based products and wheat-based products, and a method to determine total fumonisins (free and bound/hidden forms) in maize-based products. The validated multi-mycotoxin method was based on extraction with acidified acetonitrile and LC-ESI(+)-MS/MS analysis, with LOQs ranging from 0.5 to 121μg/kg, and proved to be suitable for the multi-mycotoxin analysis in wheat, maize and rice products. Bound/hidden fumonisins were determined after extraction of the free forms using the multi-mycotoxin method, followed by a basic hydrolysis of the unextracted bound/hidden and solid-liquid extraction with low temperature purification (SLE-LTP). The hydrolysis efficiency of the bound/hidden extraction procedure was investigated by analyzing a maize reference material and showed recoveries ranging from 75% (HFB2) to 108% (HFB1). The use of isotope internal standards was crucial for mycotoxins quantification in maize meal and wheat flour, while for rice, external calibration and matrix matched curves gave satisfactory results. All 55 samples of wheat-based products analyzed were contaminated with at least one mycotoxin and 16% of 44 rice samples were also contaminated. The most prevalent mycotoxins were DON and ZON in wheat-based products. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Undergraduate physics laboratory: Electrophoresis in chromatography paper

    Science.gov (United States)

    Hyde, Alexander; Batishchev, Oleg

    2015-12-01

    An experiment studying the physical principles of electrophoresis in liquids was developed for an undergraduate laboratory. We have improved upon the standard agarose gel electrophoresis experimental regime with a straightforward and cost-effective procedure, in which drops of widely available black food coloring were separated by electric field into their dye components on strips of chromatography paper soaked in a baking soda/water solution. Terminal velocities of seven student-safe dyes were measured as a function of the electric potential applied along the strips. The molecular mobility was introduced and calculated by analyzing data for a single dye. Sources of systematic and random errors were investigated.

  18. Standards not that standard.

    Science.gov (United States)

    Vilanova, Cristina; Tanner, Kristie; Dorado-Morales, Pedro; Villaescusa, Paula; Chugani, Divya; Frías, Alba; Segredo, Ernesto; Molero, Xavier; Fritschi, Marco; Morales, Lucas; Ramón, Daniel; Peña, Carlos; Peretó, Juli; Porcar, Manuel

    2015-01-01

    There is a general assent on the key role of standards in Synthetic Biology. In two consecutive letters to this journal, suggestions on the assembly methods for the Registry of standard biological parts have been described. We fully agree with those authors on the need of a more flexible building strategy and we highlight in the present work two major functional challenges standardization efforts have to deal with: the need of both universal and orthogonal behaviors. We provide experimental data that clearly indicate that such engineering requirements should not be taken for granted in Synthetic Biology.

  19. Quantification of active infliximab in human serum with liquid chromatography-tandem mass spectrometry using a tumor necrosis factor alpha -based pre-analytical sample purification and a stable isotopic labeled infliximab bio-similar as internal standard: A target-based, sensitive and cost-effective method.

    Science.gov (United States)

    El Amrani, Mohsin; van den Broek, Marcel P H; Göbel, Camiel; van Maarseveen, Erik M

    2016-07-08

    The therapeutic monoclonal antibody Infliximab (IFX) is a widely used drug for the treatment of several inflammatory autoimmune diseases. However, approximately 10% of patients develop anti-infliximab antibodies (ATIs) rendering the treatment ineffective. Early detection of underexposure to unbound IFX would result in a timely switch of therapy which could aid in the treatment of this disease. Streptavidin coated 96 well plates were used to capture biotinylated-tumor necrosis factor -alpha (b-TNF-α), which in turn was used to selectively extract the active form of IFX in human serum. After elution, IFX was digested using trypsin and one signature peptide was selected for subsequent analysis on liquid chromatography-tandem mass spectrometry (LC-MS/MS). The internal standard used was a stable isotopic labeled IFX bio-similar. The assay was successfully validated according to European Medicines Agency (EMA) guidelines and was found to be linear in a range of 0.5-20μg/mL (r(2)=0.994). Lower limit of quantification for the assay (based pre-analytical sample purification. Moreover, low volume and costs of consumables per sample promote its feasibility in (pre)clinical studies and in therapeutic drug monitoring. This method should be considered as first choice due to its accuracy and multiple degree of selectivity. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Introduction to modern liquid chromatography

    National Research Council Canada - National Science Library

    Snyder, Lloyd R; Kirkland, J. J; Dolan, John W

    2010-01-01

    "High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample...

  1. Calcium-sensitive immunoaffinity chromatography

    DEFF Research Database (Denmark)

    Henriksen, Maiken L; Lindhardt Madsen, Kirstine; Skjoedt, Karsten

    2014-01-01

    Immunoaffinity chromatography is a powerful fractionation technique that has become indispensable for protein purification and characterization. However, it is difficult to retrieve bound proteins without using harsh or denaturing elution conditions, and the purification of scarce antigens...... to homogeneity may be impossible due to contamination with abundant antigens. In this study, we purified the scarce, complement-associated plasma protein complex, collectin LK (CL-LK, complex of collectin liver 1 and kidney 1), by immunoaffinity chromatography using a calcium-sensitive anti-collectin-kidney-1 m...... chromatography was superior to the traditional immunoaffinity chromatographies and resulted in a nine-fold improvement of the purification factor. The technique is applicable for the purification of proteins in complex mixtures by single-step fractionation without the denaturation of eluted antigens...

  2. Flow Rates in Liquid Chromatography, Gas Chromatography and Supercritical Fluid Chromatography: A Tool for Optimization

    Directory of Open Access Journals (Sweden)

    Joris Meurs

    2016-08-01

    Full Text Available This paper aimed to develop a standalone application for optimizing flow rates in liquid chromatography (LC, gas chromatography (GC and supercritical fluid chromatography (SFC. To do so, Van Deemter’s equation, Knox’ equation and Golay’s equation were implemented in a MATLAB script and subsequently a graphical user interface (GUI was created. The application will show the optimal flow rate or linear velocity and the corresponding plate height for the set input parameters. Furthermore, a plot will be shown in which the plate height is plotted against the linear flow velocity. Hence, this application will give optimized flow rates for any set conditions with minimal effort.

  3. A rapid analysis of plasma/serum ethylene and propylene glycol by headspace gas chromatography

    National Research Council Canada - National Science Library

    Ehlers, Alexandra; Morris, Cory; Krasowski, Matthew D

    2013-01-01

    A rapid headspace-gas chromatography (HS-GC) method was developed for the analysis of ethylene glycol and propylene glycol in plasma and serum specimens using 1,3-propanediol as the internal standard...

  4. Electrochemical oxidation and protein adduct formation of aniline: a liquid chromatography/mass spectrometry study.

    Science.gov (United States)

    Melles, Daniel; Vielhaber, Torsten; Baumann, Anne; Zazzeroni, Raniero; Karst, Uwe

    2012-04-01

    Historically, skin sensitization tests are typically based on in vivo animal tests. However, for substances used in cosmetic products, these tests have to be replaced according to the European Commission regulation no. 1223/2009. Modification of skin proteins by electrophilic chemicals is a key process associated with the induction of skin sensitization. The present study investigates the capabilities of a purely instrumental setup to determine the potential of commonly used non-electrophilic chemicals to cause skin sensitization by the generation of electrophilic species from the parent compound. In this work, the electrophiles were generated by the electrochemical oxidation of aniline, a basic industrial chemical which may also be released from azo dyes in cosmetics. The compound is a known sensitizer and was oxidized in an electrochemical thin-layer cell which was coupled online to electrospray ionization-mass spectrometry. The electrochemical oxidation was performed on a boron-doped diamond working electrode, which is able to generate hydroxyl radicals in aqueous solutions at high potentials. Without any pretreatment, the oxidation products were identified by electrospray ionization/time-of-flight mass spectrometry (ESI-ToF-MS) using their exact masses. A mass voltammogram was generated by plotting the obtained mass spectra against the applied potential. Oligomerization states with up to six monomeric units in different redox states of aniline were observed using this setup. This approach was extended to generate adducts between the oxidation products of aniline and the tripeptide glutathione. Two adducts were identified with this trapping experiment. Protein modification was carried out subsequently: Aniline was oxidized at a constant potential and was allowed to react with β-lactoglobulin A (β-LGA) or human serum albumin (HSA), respectively. The generated adducts were analyzed by liquid chromatography coupled to ESI-ToF-MS. For both β-LGA and HSA, aniline

  5. Enantioselective high performance liquid chromatography and supercritical fluid chromatography separation of spirocyclic terpenoid flavor compounds.

    Science.gov (United States)

    Schaffrath, Mathias; Weidmann, Verena; Maison, Wolfgang

    2014-10-10

    Chiral spirocyclic terpenoids are abundant natural flavors with significant impact particularly on the food industry. Chromatographic methods for analytical and preparative separation of these compounds are therefore of high interest to natural product chemists in academia and industry. Gas chromatography on chiral stationary phases is currently the standard method for the separation of volatile terpenoids, limiting the scale to analytical quantities. We report herein high performance liquid chromatography (HPLC) and supercritical fluid chromatography (SFC) protocols for the chiral separation of several racemic spirocyclic terpenoids such as the important flavors theaspirane and vitispirane. A screening of mobile phases and 16 commercially available chiral stationary phases (CSPs) largely based on polysaccharides led to identification of protocols for the separation of all terpenoids tested. SFC methods were found to be particularly useful for the separation of these spirocyclic flavors due to the volatility and low polarity of the compounds. The reported chiral HPLC and SFC protocols are scalable alternatives to gas chromatographic separations of volatile terpenoid flavors. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Stability of thin layer electrodeposited copper in solid polymer electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Atchia, S. (Lab. d' Ionique et d' Electrochimie des Solides de Grenoble, I.N.P.G.-E.N.S.E.E.G., 38 - St. Martin d' Heres (France)); Deroo, D. (Lab. d' Ionique et d' Electrochimie des Solides de Grenoble, I.N.P.G.-E.N.S.E.E.G., 38 - St. Martin d' Heres (France)); Petit, J.P. (Lab. d' Ionique et d' Electrochimie des Solides de Grenoble, I.N.P.G.-E.N.S.E.E.G., 38 - St. Martin d' Heres (France)); Armand, M. (Lab. d' Ionique et d' Electrochimie des Solides de Grenoble, I.N.P.G.-E.N.S.E.E.G., 38 - St. Martin d' Heres (France)); Rosman, N. (Lab. d' Ionique et d' Electrochimie des Solides de Grenoble, I.N.P.G.-E.N.S.E.E.G., 38 - St. Martin d' Heres (France))

    1993-03-01

    In the course of our studies on variable reflection windows involving copper deposition, we have proposed to use P(EO)[sub n]KCu[sub x]I[sub 1+x] complexes. The excess I[sup -] ions stabilizes copper (I) through formation of CuI[sub n+1][sup n-] and the transport of copper is solely due to the diffusion of anionic complexes which acts as copper vehicles. Copper electrodeposition has been observed. The stripping of the copper layers strongly depends upon the relaxation time between the copper plating and the beginning of the anodic voltametric scan. The copper deposit slowly vanishes with time. A cathodic current is observed before the copper plating process which we relate to the possible reduction of an oxidizing species present in the electrolyte. The search for such oxidizing species (Cu[sup 2+], I[sub 3][sup -]) has been made using ESR and Raman spectroscopy and we have shown the presence of I[sub 3][sup -]. (orig.)

  7. Development and validation of a thin layer chromatographic method ...

    African Journals Online (AJOL)

    The two drugs were satisfactorily resolved with mean Rf values of 0.04 ± 0.03 and 0.06 ± 0.07 for artesunate and amodiaquine, respectively. The accuracy and reliability of the method was assessed by evaluation of linearity (0.001 – 6.0 and 0.05 – 6.0 mg/ml for artesunate and amodiaquine), precision (intraday RSD 10.68 ...

  8. Physicochemical, thin layer and gas-liquid chromatographic ...

    African Journals Online (AJOL)

    DELL

    2012-05-22

    May 22, 2012 ... boiling and was titrated with 0.1 N KOH solutions using phenolphthalein as indicator. Iodine value. Iodine value is the measure of the unsaturation of oils and is expressed as the number of grams of iodine absorbed by 100 g of an oil. After dissolving the flower oil (0.1158 g) in 15 ml of CCl4, 25 ml of Wijs' ...

  9. EFFECT OF OPERATING CONDITIONS ON THIN LAYERS OF ...

    African Journals Online (AJOL)

    1Laboratoire des énergies nouvelles et renouvelables, Université de Ouargla, Algérie. 2Unité de recherche ... avec une haute pression d'argon et une énergie remarquable des atomes arrachés, dans le cas de la ... vitesses plus importantes de la consommation de titane et de la formation de carbure de titane TiC que ...

  10. Saturn's rings - Particle size distributions for thin layer model

    Science.gov (United States)

    Zebker, H. A.; Marouf, E. A.; Tyler, G. L.

    1985-01-01

    A model incorporating limited interaction between the incident energy and particles in the ring is considered which appears to be consistent with the multiple scattering process in Saturn's rings. The model allows for the small physical thickness of the rings and can be used to relate Voyager 1 observations of 3.6- and 13-cm wavelength microwave scatter from the rings to the ring particle size distribution function for particles with radii ranging from 0.001 to 20 m. This limited-scatter model yields solutions for particle size distribution functions for eight regions in the rings, which exhibit approximately inverse-cubic power-law behavior.

  11. BAlN thin layers for deep UV applications

    Energy Technology Data Exchange (ETDEWEB)

    Li, Xin; Voss, Paul L.; Ougazzaden, Abdallah [School of Electrical and Computer Engineering, Georgia Institute of Technology, Metz (France); UMI 2958, Georgia Tech-CNRS, Metz (France); Sundaram, Suresh; El Gmili, Youssef; Moudakir, Tarik [UMI 2958, Georgia Tech-CNRS, Metz (France); Genty, Frederic [Supelec, LMOPS, EA 4423, Metz (France); Bouchoule, Sophie; Patriarche, Gilles [LPN CNRS, UPR20, Marcoussis (France); Dupuis, Russell D. [Center for Compound Semiconductors and School of Electrical and Computer Engineering, Georgia Institute of Technology, Atlanta, GA (United States); Salvestrini, Jean-Paul [UMI 2958, Georgia Tech-CNRS, Metz (France); Universite de Lorraine, LMOPS, EA 4423, Metz (France)

    2015-04-01

    In this work, wurtzite BAlN layers with boron composition as high as 12% were successfully grown by MOVPE. The growth was performed at 650 C and then annealed at 1020 C. Low temperature growth was used in order to alleviate B-rich phase poisoning under high TEB/III ratio. The growth was performed by continuous epitaxy as well as by flow-modulate epitaxy. BAlN single layers with clearly defined X-ray diffraction peaks were achieved on AlN templates which are appropriate substrates for deep UV devices, as well as on GaN templates to facilitate distinguishing of the XRD peak of BAlN from the substrate peak. The layer demonstrated columnar crystalline features and inherited wurtzite structure from substrates. Cross-section STEM image (bright field) of 75 nm thick BAlN layers containing 12% boron taken along the [11-2 0] zone axis. Zone A is lattice-oriented along c-axis and zone B has columnar structure; (b) higher magnification image for the top part of the layer; (c) higher magnification image for the film/substrate interface. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  12. Characterization of pulsed laser deposited chalcogenide thin layers

    Energy Technology Data Exchange (ETDEWEB)

    Petkova, T. [Institute of Electrochemistry and Energy Systems (IEES), Bulgarian Academy of Sciences, Sofia (Bulgaria)], E-mail: tpetkova@bas.bg; Popov, C. [Institute of Nanostructure Technologies and Analytics (INA), University of Kassel (Germany); Hineva, T.; Petkov, P. [Laboratory of Thin Film Technology, Department of Physics, University of Chemical Technology and Metallurgy, Sofia (Bulgaria); Socol, G.; Axente, E.; Mihailescu, C.N.; Mihailescu, I.N. [National Institute for Lasers, Plasma, and Radiation Physics, Bucharest-Magurele (Romania); Reithmaier, J.P. [Institute of Nanostructure Technologies and Analytics (INA), University of Kassel (Germany)

    2009-03-01

    In this work we report on pulsed laser deposition (PLD) of chalcogenide thin films from the systems (AsSe){sub 100-x}AgI{sub x} and (AsSe){sub 100-x}Ag{sub x} for sensing applications. A KrF* excimer laser ({lambda} = 248 nm; {tau}{sub FWHM} = 25 ns) was used to ablate the targets that had been prepared from the synthesised chalcogenide materials. The films were deposited in either vacuum (4 x 10{sup -4} Pa) or argon (5 Pa) on silicon and glass substrates kept at room temperature. The basic properties of the films, including their morphology, topography, structure, and composition were characterised by complementary techniques. Investigations by X-ray diffraction (XRD) confirmed the amorphous nature of the films, as no strong diffraction reflections were found. The film composition was studied by energy dispersive X-ray (EDX) spectroscopy. The morphology of the films investigated by scanning electron microscopy (SEM), revealed a particulate-covered homogeneous surface, typical of PLD. Topographical analyses by atomic force microscopy (AFM) showed that the particulate size was slightly larger in Ar than in vacuum. The uniform surface areas were rather smooth, with root mean square (rms) roughness increasing up to several nanometers with the AgI or Ag doping. Based upon the results from the comprehensive investigation of the basic properties of the chalcogenide films prepared by PLD and their dependence on the process parameters, samples with appropriate sorption properties can be selected for possible applications in cantilever gas sensors.

  13. Thin layers of YSZ and GDC electrolytes deposited by RSDT

    Energy Technology Data Exchange (ETDEWEB)

    Neagu, R.; Maric, R.; Deces-Petit, C. [National Research Council of Canada, Vancouver, BC (Canada). Inst. for Fuel Cell Innovation

    2009-07-01

    The reactive spray deposition technique (RSDT) is a flame-based deposition and powder production process that uses the combustion of solvents and precursors to create a deposition plume. The plume can be conducted from the vapour phase, and the plume's temperature can be adjusted to condensate the vapors into particles. Ceramic layers can also be deposited directly from the vapor phase. This study used the RSDT technique to synthesize thin electrolyte layers for solid oxide fuel cells (SOFCs). Yttria-stabilized zircon (YSZ) and GDC layers were deposited on anode substrates and Si wafers. Scanning electron microscopy (SEM) was used to analyze the coating microstructures. Phase structure and composition were analyzed using X-ray diffraction and energy-dispersive X-ray spectroscopy (EDX). Electrochemical measurements were conducted to determine electrolyte properties. Results of the analyses showed that the thin coatings showed good conductivity and stability. Additional research is underway to use the RSDT technique in larger scale applications.

  14. Thin Layer Drying Kinetics of Pineapple: Effect of Blanching ...

    African Journals Online (AJOL)

    Biochemical Engineering and Biotechnology Research Laboratory, Department of Chemical Engineering,. Ladoke Akintola University of Technology, Ogbomoso. Nigeria. [*Corresponding ... 1996; Pangavhane et al., 1999; Doymaz and Pala,. 2002; Doymaz, 2004). Although pineapples are one of the world's most traded ...

  15. Total absorption of electromagnetic waves in ultimately thin layers

    CERN Document Server

    Ra'di, Younes; Tretyakov, Sergei A

    2012-01-01

    We consider single-layer arrays of electrically small lossy bi-anisotropic particles that completely absorb electromagnetic waves at normal incidence. Required conditions for electromagnetic properties of bi-anisotropic particles have been identified in the most general case of uniaxial reciprocal and nonreciprocal particles. We consider the design possibilities offered by the particles of all four fundamental classes of bianisotropic inclusions: reciprocal chiral and omega particles and nonreciprocal Tellegen and moving particles. We also study the reflection/transmission properties of asymmetric structures with different properties when illuminated from the opposite sides of the sheet. It has been found that it is possible to realize single-layer grids which exhibit the total absorption property when illuminated from one side but are totally transparent when illuminated from the other side (an ultimately thin isolator). Other possible properties are co-polarized or twist polarized reflection from the side o...

  16. Charged particle detectors made from thin layers of amorphous silicon

    Energy Technology Data Exchange (ETDEWEB)

    Morel, J.R.

    1986-05-01

    A series of experiments was conducted to determine the feasibility of using hydrogenated amorphous silicon (..cap alpha..-Si:H) as solid state thin film charged particle detectors. /sup 241/Am alphas were successfully detected with ..cap alpha..-Si:H devices. The measurements and results of these experiments are presented. The problems encountered and changes in the fabrication of the detectors that may improve the performance are discussed.

  17. Physicochemical, thin layer and gas-liquid chromatographic ...

    African Journals Online (AJOL)

    DELL

    2012-05-22

    May 22, 2012 ... sodium (693.68), potassium (629.25), iron (253.04), nickel (2.17), zinc (24.28), copper (23.24) and lead ... Recently, volatile chemical components of ..... of mango var. Ataulfo characterized by SPME and capillary GC/MS spectroscopy, J. Mex. Chem. Soc. 51(3): 145-147. Severi JA, Lima ZP, Kushima H, ...

  18. Thin Layer Drying Kinetics of Pineapple: Effect of Blanching ...

    African Journals Online (AJOL)

    The results show that drying rates and drying times were affected by the blanching temperature-time combinations. Drying times increased as blanching temperature-time combinations increased. The predominant drying regime of the blanched pineapple was observed to be in the falling rate period. The logarithmic model ...

  19. NUMERICAL SIMULATION OF THIN LAYER COFFEE DRYING BY CONTROL VOLUMES

    Directory of Open Access Journals (Sweden)

    HÉCTOR J. CIRO-VELÁSQUEZ

    2010-01-01

    Full Text Available El modelo de secado en capa delgada desarrollado por Sokhansanj y Bruce (1987 fue implementado para simular el secado de un grano de café pergamino. El modelo computacional fue definido en estado transitorio y unidimensional para una esfera de radio equivalente utilizando la técnica del volumen de control. Los resultados indicaron que el valor numérico del coeficiente de transferencia de masa es muy pequeño (orden de magnitud alrededor de 10 7 m/s haciendo que la predicción del contenido de humedad sea muy sensible a este valor. Además, los resultados de la simulación mostraron que la predicción del modelo numérico fue favorablemente similar a los datos experimentales dados en la literatura.

  20. Buckling instability of a thin-layer rectilinear Couette flow

    CERN Document Server

    Slim, Anja; Mahadevan, L

    2011-01-01

    We analyse the buckling stability of a thin, viscous sheet when subject to simple shear, providing conditions for the onset of the dominant out-of-plane modes using two models: (i) an asymptotic theory for the dynamics of a viscous plate and (ii) the full Stokes equations. In either case, the plate is stabilised by a combination of viscous resistance, surface tension and buoyancy relative to an underlying denser fluid. In the limit of vanishing thickness, plates buckle at a shear rate $\\gamma/(\\mu d)$ independent of buoyancy, where 2d is the plate thickness, $\\gamma$ is the average surface tension between the upper and lower surfaces and $\\mu$ is the fluid viscosity. For thicker plates stabilised by an equal surface tension at the upper and lower surfaces, at and above onset, the most unstable mode has moderate wavelength, is stationary in the frame of the centre-line, spans the width of the plate with crests and troughs aligned at approximately $45^\\circ$ to the walls and closely resembles elastic shear mode...