Isolation of Three Components from Spearmint Oil: An Exercise in Column and Thin-Layer Chromatography

ERIC Educational Resources Information Center

Davies, Don R.; Johnson, Todd M.

2007-01-01

A simple experiment for undergraduate organic chemistry students to separate a colorless mixture using column chromatography and then monitor the outcome of the separation using thin-layer chromatography (TLC) and infrared spectroscopy(IR) is described. The experiment teaches students the principle and techniques of column and thin-layer…

Use of low volatility mobile phases in electroosmotic thin-layer chromatography.

PubMed

Berezkin, V G; Balushkin, A O; Tyaglov, B V; Litvin, E F

2005-08-19

A variant of electroosmotic thin-layer chromatography is suggested with the use of low volatility compounds as mobile phases aimed at drastically decreasing the evaporation of the mobile phase and improving the reproducibility of the method. The linear movement velocity of zones of separated compounds is experimentally shown to increase 2-12-fold in electroosmotic chromatography (compared to similar values in traditional TLC). The separation efficiency is also considerably increased.

A Simple and Inexpensive Capillary Holder for Thin-Layer Chromatography

ERIC Educational Resources Information Center

Pintea, Beniamin-Nicolae V.

2011-01-01

Thin-layer chromatography (TLC) is a widely used method of qualitative analysis in organic synthesis, as it uniquely combines low cost, rapidity, simplicity, versatility, small quantities of sample and low detection limits. The simplest and most economical method for the application of samples onto TLC plates is by hand, using glass capillaries.…

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

DOEpatents

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.

Comprehensive thin-layer chromatography mass spectrometry of flavanols from Juniperus communis L. and Punica granatum L.

PubMed

Smrke, Samo; Vovk, Irena

2013-05-10

The coupling of thin-layer chromatography with mass spectrometry (TLC-MS) for the analysis of monomeric flavanols and proanthocyanidins in samples presented as complex matrices has been studied. The elution conditions for TLC-MS were optimised and full scans were compared with selected reaction monitoring for the MS detection of compounds. The performance of silica gel and cellulose plates with different developing solvents in TLC-MS was assessed. Cellulose plates provided superior sensitivity while ionisation suppression was encountered with silica plates. The use of a HILIC guard column beyond the elution head was found to facilitate detection of monomer compounds on silica plates. A new comprehensive TLC×MS procedure for screening flavanols in the entire chromatogram was developed as an alternative to the use of 4-dimethylaminocinnamaldehyde to determine the locations of compounds on the plate. This new procedure was applied to detect flavanols in the peel of Punica granatum L. fruits and in seeds of Juniperus communis L., in which flavanols and proanthocyanidin dimers and trimers were detected for the first time. Copyright © 2013 Elsevier B.V. All rights reserved.

Hand portable thin-layer chromatography system

DOEpatents

Haas, Jeffrey S.; Kelly, Fredrick R.; Bushman, John F.; Wiefel, Michael H.; Jensen, Wayne A.

2000-01-01

A hand portable, field-deployable thin-layer chromatography (TLC) unit and a hand portable, battery-operated unit for development, illumination, and data acquisition of the TLC plates contain many miniaturized features that permit a large number of samples to be processed efficiently. The TLC unit includes a solvent tank, a holder for TLC plates, and a variety of tool chambers for storing TLC plates, solvent, and pipettes. After processing in the TLC unit, a TLC plate is positioned in a collapsible illumination box, where the box and a CCD camera are optically aligned for optimal pixel resolution of the CCD images of the TLC plate. The TLC system includes an improved development chamber for chemical development of TLC plates that prevents solvent overflow.

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

Code of Federal Regulations, 2012 CFR

2012-04-01

... 21 Food and Drugs 8 2012-04-01 2012-04-01 false Thin-layer chromatography system for clinical use. 862.2270 Section 862.2270 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES CLINICAL CHEMISTRY AND CLINICAL TOXICOLOGY DEVICES Clinical Laboratory...

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

Code of Federal Regulations, 2013 CFR

2013-04-01

... 21 Food and Drugs 8 2013-04-01 2013-04-01 false Thin-layer chromatography system for clinical use. 862.2270 Section 862.2270 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES CLINICAL CHEMISTRY AND CLINICAL TOXICOLOGY DEVICES Clinical Laboratory...

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

Code of Federal Regulations, 2014 CFR

2014-04-01

... 21 Food and Drugs 8 2014-04-01 2014-04-01 false Thin-layer chromatography system for clinical use. 862.2270 Section 862.2270 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN SERVICES (CONTINUED) MEDICAL DEVICES CLINICAL CHEMISTRY AND CLINICAL TOXICOLOGY DEVICES Clinical Laboratory...

Analysis and Identification of Acid-Base Indicator Dyes by Thin-Layer Chromatography

ERIC Educational Resources Information Center

Clark, Daniel D.

2007-01-01

Thin-layer chromatography (TLC) is a very simple and effective technique that is used by chemists by different purposes, including the monitoring of the progress of a reaction. TLC can also be easily used for the analysis and identification of various acid-base indicator dyes.

A reversed-phase compatible thin-layer chromatography autography for the detection of acetylcholinesterase inhibitors.

PubMed

Ramallo, I Ayelen; García, Paula; Furlan, Ricardo L E

2015-11-01

A dual readout autographic assay to detect acetylcholinesterase inhibitors present in complex matrices adsorbed on reversed-phase or normal-phase thin-layer chromatography plates is described. Enzyme gel entrapment with an amphiphilic copolymer was used for assay development. The effects of substrate and enzyme concentrations, pH, incubation time, and incubation temperature on the sensitivity and the detection limit of the assay were evaluated. Experimental design and response surface methodology were used to optimize conditions with a minimum number of experiments. The assay allowed the detection of 0.01% w/w of physostigmine in both a spiked Sonchus oleraceus L. extract chromatographed on normal phase and a spiked Pimenta racemosa (Mill.) J.W. Moore leaf essential oil chromatographed on reversed phase. Finally, the reversed-phase thin-layer chromatography assay was applied to reveal the presence of an inhibitor in the Cymbopogon citratus (DC.) Stapf essential oil. The developed assay is able to detect acetylcholinesterase inhibitors present in complex matrixes that were chromatographed in normal phase or reversed-phase thin-layer chromatography. The detection limit for physostigmine on both normal and reversed phase was of 1×10(-4) μg. The results can be read by a change in color and/or a change in fluorescence. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

Valle, Demetrio L; Puzon, Juliana Janet M; Cabrera, Esperanza C; Rivera, Windell L

2016-01-01

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 R f 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 R f 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 R f 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(trifluoromethyl)phosphine, heptafluorobutyrate, 3-fluoro-2-propynenitrite, 4-(2-propenyl)phenol, 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.

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

PubMed Central

Valle, Demetrio L.; Puzon, Juliana Janet M.; Cabrera, Esperanza C.

2016-01-01

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 R f 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 R f 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 R f 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(trifluoromethyl)phosphine, heptafluorobutyrate, 3-fluoro-2-propynenitrite, 4-(2-propenyl)phenol, 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. PMID:27478476

Thin-layer chromatography and mass spectrometry coupled using proximal probe thermal desorption with electrospray or atmospheric pressure chemical ionization.

PubMed

Ovchinnikova, Olga S; Van Berkel, Gary J

2010-06-30

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.

Analysis of Peppermint Leaf and Spearmint Leaf Extracts by Thin-Layer Chromatography

ERIC Educational Resources Information Center

Pelter, Libbie S. W.; Amico, Andrea; Gordon, Natalie; Martin, Chylah; Sandifer, Dessalyn; Pelter, Michael W.

2008-01-01

In this inquiry-based activity, the usefulness of thin-layer chromatography (TLC) to visualize the difference between spearmint and peppermint is explored. The experiment may be used in any class where TLC is discussed from high school to college. We have used this activity with science majors in an organic chemistry laboratory, with non-science…

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.

PubMed

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.

Quantitative analysis of psilocybin and psilocin in psilocybe baeocystis (Singer and Smith) by high-performance liquid chromatography and by thin-layer chromatography.

PubMed

Beug, M W; Bigwood, J

1981-03-27

Rapid quantification of psilocybin and psilocin in extracts of wild mushrooms is accomplished by reversed-phase high-performance liquid chromatography with paired-ion reagents. Nine solvent systems and three solid supports are evaluated for their efficiency in separating psilocybin, psilocin and other components of crude mushroom extracts by thin-layer chromatography.

Purification of pharmaceutical preparations using thin-layer chromatography to obtain mass spectra with Direct Analysis in Real Time and accurate mass spectrometry.

PubMed

Wood, Jessica L; Steiner, Robert R

2011-06-01

Forensic analysis of pharmaceutical preparations requires a comparative analysis with a standard of the suspected drug in order to identify the active ingredient. Purchasing analytical standards can be expensive or unattainable from the drug manufacturers. Direct Analysis in Real Time (DART™) is a novel, ambient ionization technique, typically coupled with a JEOL AccuTOF™ (accurate mass) mass spectrometer. While a fast and easy technique to perform, a drawback of using DART™ is the lack of component separation of mixtures prior to ionization. Various in-house pharmaceutical preparations were purified using thin-layer chromatography (TLC) and mass spectra were subsequently obtained using the AccuTOF™- DART™ technique. Utilizing TLC prior to sample introduction provides a simple, low-cost solution to acquiring mass spectra of the purified preparation. Each spectrum was compared against an in-house molecular formula list to confirm the accurate mass elemental compositions. Spectra of purified ingredients of known pharmaceuticals were added to an in-house library for use as comparators for casework samples. Resolving isomers from one another can be accomplished using collision-induced dissociation after ionization. Challenges arose when the pharmaceutical preparation required an optimized TLC solvent to achieve proper separation and purity of the standard. Purified spectra were obtained for 91 preparations and included in an in-house drug standard library. Primary standards would only need to be purchased when pharmaceutical preparations not previously encountered are submitted for comparative analysis. TLC prior to DART™ analysis demonstrates a time efficient and cost saving technique for the forensic drug analysis community. Copyright © 2011 John Wiley & Sons, Ltd. Copyright © 2011 John Wiley & Sons, Ltd.

What Factors Affect the Separation of Substances Using Thin-Layer Chromatography? An Undergraduate Experiment.

ERIC Educational Resources Information Center

Nash, John J.; Meyer, Jeanne A.; Everson, Barbara

2001-01-01

Rx values in thin-layer chromatography (TLC) depend strongly on the solvent saturation of the atmosphere above the liquid in the TLC developing chamber. Presents an experiment illustrating the potentially dramatic effects on TLC Rx values of not equilibrating the solvent atmosphere during development. (ASK)

The offline combination of thin-layer chromatography and high-performance liquid chromatography with diode array detection and micrOTOF-Q mass spectrometry for the separation and identification of spinochromes from sea urchin (Strongylocentrotus droebachiensis) shells.

PubMed

Shikov, Alexander N; Ossipov, Vladimir I; Martiskainen, Olli; Pozharitskaya, Olga N; Ivanova, Svetlana A; Makarov, Valery G

2011-12-16

Thin-layer chromatography (TLC) with off-line high-performance liquid chromatography coupled to diode array detection and micrOTOF-Q mass spectrometry (HPLC-DAD-MS) resulted in the successful fractionation, separation and identification of spinochrome pigments from sea urchin (Strongylocentrotus droebachiensis) shells. Two fractions of pigments were separated by TLC and eluted with methanol using a TLC-MS interface. HPLC-DAD-MS analysis of the fractions indicated the presence of six sea urchin pigments: spinochrome monomers B and D, three spinochrome dimers (anhydroethylidene-6,6'-bis(2,3,7-trihydroxynaphthazarin) and its isomer and ethylidene-6,6'-bis(2,3,7-trihydroxynaphthazarin)), and one pigment that was preliminary identified as a spinochrome dimer with the structural formula C(22)H(16)O(16). Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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.

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

PubMed

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.

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

PubMed Central

Doshi, Gaurav Mahesh; Une, Hemant Devidas

2016-01-01

Objective: 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. Materials and Methods: 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. Results: 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. Conclusion: The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. SUMMARY 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 PMID:26941534

Evaluating Mechanisms of Dihydroxylation by Thin-Layer Chromatography: A Microscale Experiment for Organic Chemistry

ERIC Educational Resources Information Center

Burlingham, Benjamin T.; Rettig, Joseph C.

2008-01-01

A microscale experiment is presented in which cyclohexene is dihydroxylated under three sets of conditions: epoxidation-hydrolysis, permanganate oxidation, and the Woodward dihydroxylation. The products of the reactions are determined by the use of thin-layer chromatography. Teams of students are presented with proposed mechanisms for each…

Phospholipids, Dietary Supplements, and Chicken Eggs: An Inquiry-Based Exercise Using Thin-Layer Chromatography

ERIC Educational Resources Information Center

Potteiger, Sara E.; Belanger, Julie M.

2015-01-01

This inquiry-based experiment is designed for organic or biochemistry undergraduate students to deduce the identity of phospholipids extracted from chicken eggs and dietary supplements. This is achieved using thin-layer chromatography (TLC) data, a series of guided questions of increasing complexity, and provided relative retention factor (Rf)…

Detection and determination of organophosphorus insecticides in tissues by thin-layer chromatography.

PubMed

Tewari, S N; Harpalani, S P

1977-01-11

The toxicological analysis of 12 common organophosphorus insecticides is described. Suitable methods for the extraction of organophosphorus insecticides from tissues are proposed. The detection, identification and estimation of these insecticides by thin-layer chromatography is described for 25 solvent systems and a series of chromogenic reagents. The distribution of insecticides in human body tissues in five cases of poisoning by ethyl parathion, malathion, dimethoate, sumithion and phosphamidon has also been studied.

Determination of Absolute Configuration of Secondary Alcohols Using Thin-Layer Chromatography

PubMed Central

Wagner, Alexander J.; Rychnovsky, Scott D.

2013-01-01

A new implementation of the Competing Enantioselective Conversion (CEC) method was developed to qualitatively determine the absolute configuration of enantioenriched secondary alcohols using thin-layer chromatography. The entire process for the method requires approximately 60 min and utilizes micromole quantities of the secondary alcohol being tested. A number of synthetically relevant secondary alcohols are presented. Additionally, 1H NMR spectroscopy was conducted on all samples to provide evidence of reaction conversion that supports the qualitative method presented herein. PMID:23593963

Combining surface enhanced Raman scattering (SERS) and high-performance thin-layer chromatography (HPTLC)

NASA Astrophysics Data System (ADS)

Koglin, E.

A new method for preparing SERS active surfaces using silver colloidal spheres deposited on HPTLC plates, used for thin-layer chromatography, is discussed in detail. The sensitivity of these activated HPTLC plates is so high that in-situ vibrational investigations of chromatogram spots are possible at the nanogram level. The HPTLC/SERS spectra of purine, benzoic acid and 1-nitro-pyrene adsorbed on silver colloidal activated silica gel plates are measured in the nanogram region. In addition we also report in this paper on the results of a feasibility study performed to evaluate the analytical potential of micro-Raman spectroscopy (triple monochromator, multichannel detection system) in SERS/HPTLC spot characterization. It permits the acquisition of Raman spectra from HPTLC spots down to 1 μm in size or other forms of microsamples approaching the picogram level in mass.

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

PubMed

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.

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.

PubMed

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.

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.

PubMed

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

Analysis of biodiesel and biodiesel-petrodiesel blends by high performance thin layer chromatography combined with easy ambient sonic-spray ionization mass spectrometry.

PubMed

Eberlin, Livia S; Abdelnur, Patricia V; Passero, Alan; de Sa, Gilberto F; Daroda, Romeu J; de Souza, Vanderlea; Eberlin, Marcos N

2009-08-01

High performance thin layer chromatography (HPTLC) combined with on-spot detection and characterization via easy ambient sonic-spray ionization mass spectrometry (EASI-MS) is applied to the analysis of biodiesel (B100) and biodiesel-petrodiesel blends (BX). HPTLC provides chromatographic resolution of major components whereas EASI-MS allows on-spot characterization performed directly on the HPTLC surface at ambient conditions. Constituents (M) are detected by EASI-MS in a one component-one ion fashion as either [M + Na](+) or [M + H](+). For both B100 and BX samples, typical profiles of fatty acid methyl esters (FAME) detected as [FAME + Na](+) ions allow biodiesel typification. The spectrum of the petrodiesel spot displays a homologous series of protonated alkyl pyridines which are characteristic for petrofuels (natural markers). The spectrum for residual or admixture oil spots is characterized by sodiated triglycerides [TAG + Na](+). The application of HPTLC to analyze B100 and BX samples and its combination with EASI-MS for on-spot characterization and quality control is demonstrated.

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

PubMed

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.

In situ identification of high-performance thin-layer chromatography spots by fourier transform surface-enhanced Raman scattering

NASA Astrophysics Data System (ADS)

Koglin, Eckhardt; Kramer, Hella; Sawatski, Juergen; Lehner, Carolin; Hellman, Janice L.

1994-01-01

FT-SERS has been used to identify samples supported on high-performance thin-layer chromatography plates. The TLC plates were sprayed with colloidal silver solutions which resulted in enhancement of the FT-Raman scattering of these biologically and environmentally important compounds.

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

ERIC Educational Resources Information Center

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…

High Performance Thin layer Chromatography: Densitometry Method for Determination of Rubraxanthone in the Stem Bark Extract of Garcinia cowa Roxb.

PubMed

Hamidi, Dachriyanus; Aulia, Hilyatul; Susanti, Meri

2017-01-01

Garcinia cowa is a medicinal plant widely grown in Southeast Asia and tropical countries. Various parts of this plant have been used in traditional folk medicine. The bark, latex, and root have been used as an antipyretic agent, while fruit and leaves have been used as an expectorant, for indigestion and improvement of blood circulation. This study aims to determine the concentration of rubraxanthone found in ethyl acetate extract of the stem bark of G. cowa by the high-performance thin-layer chromatography (HPTLC). HPTLC method was performed on precoated silica gel G 60 F254 plates using an HPTLC system with a developed mobile-phase system of chloroform: ethyl acetate: methanol: formic acid (86:6:3:5). A volume of 5 μL of standard and sample solutions was applied to the chromatographic plates. The plates were developed in saturated mode of twin trough chamber at room temperature. The method was validated based on linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and specificity. The spots were observed at ultraviolet 243 nm. The linearity of rubraxanthone was obtained between 52.5 and 157.5 ppm/spot. The LOD and LOQ were found to be 4.03 and 13.42 ppm/spot, respectively. The proposed method showed good linearity, precision, accuracy, and high sensitivity. Therefore, it may be applied for the quantification of rubraxanthone in ethyl acetate extract of the stem bark of G. cowa . High performance thin layer chromatography (HPTLC) method provides rapid qualitative and quantitative estimation of rubraxanthone as a marker com¬pound in G. cowa extract used for commercial productRubraxanthone found in ethyl acetate extracts of G. cowa was successfully quantified using HPTLC method. Abbreviations Used : TLC: Thin-layer chromatography, HPTLC: High-performance thin-layer chromatography, LOD: Limit of detection, LOQ: Limit of quantification, ICH: International Conference on Harmonization.

Rapid and selective determination of multi-sulfonamides by high-performance thin layer chromatography coupled to fluorescent densitometry and electrospray ionization mass detection.

PubMed

Chen, Yisheng; Schwack, Wolfgang

2014-02-28

In the European Union (EU), sulfonamides are among the most widely administrated groups of antibiotics in animal husbandry. Therefore, monitoring their residues in edible animal tissues plays an important role in the EU food safety framework. In this work, a simple and efficient method for the rapid screening of twelve prior sulfonamides frequently prescribed as veterinary drugs by high-performance thin-layer chromatography (HPTLC) was established. Sample extracts obtained with acetonitrile were tenfold concentrated and applied to HPTLC without any further cleanup. Following separation and fluram derivatization, sensitive and selective quantitation of the analytes can readily be accomplished with fluorescent densitometry. Limits of detection and quantitation were 15-40 and 35-70μg/kg, respectively. Additionally, a confirmative detection by HPTLC-electrospray ionization mass spectrometry (HPTLC-ESI/MS) was optimized, offering straightforward identification of target zones. Therefore, the risk of potential false positive findings can efficiently be reduced. The method was validated to meet the enforced commission regulation (EU) No. 37/2010, regarding different matrix complexities (bovine milk, porcine liver and kidney). Copyright © 2014 Elsevier B.V. All rights reserved.

Bacterial Cell Wall Precursor Phosphatase Assays Using Thin-layer Chromatography (TLC) and High Pressure Liquid Chromatography (HPLC).

PubMed

Pazos, Manuel; Otten, Christian; Vollmer, Waldemar

2018-03-20

Peptidoglycan encases the bacterial cytoplasmic membrane to protect the cell from lysis due to the turgor. The final steps of peptidoglycan synthesis require a membrane-anchored substrate called lipid II, in which the peptidoglycan subunit is linked to the carrier lipid undecaprenol via a pyrophosphate moiety. Lipid II is the target of glycopeptide antibiotics and several antimicrobial peptides, and is degraded by 'attacking' enzymes involved in bacterial competition to induce lysis. Here we describe two protocols using thin-layer chromatography (TLC) and high pressure liquid chromatography (HPLC), respectively, to assay the digestion of lipid II by phosphatases such as Colicin M or the LXG toxin protein TelC from Streptococcus intermedius . The TLC method can also monitor the digestion of undecaprenyl (pyro)phosphate, whereas the HPLC method allows to separate the di-, mono- or unphosphorylated disaccharide pentapeptide products of lipid II.

Detection of mycoloylglycerol by thin-layer chromatography as a tool for the rapid inclusion of corynebacteria of clinical origin in the genus Corynebacterium.

PubMed

Yagüe, G; Segovia, M; Valero-Guillén, P L

2000-01-28

A chemotaxonomic study of some corynebacteria isolated from clinical samples revealed characteristic thin-layer chromatographic patterns for meso-diaminopimelic acid containing species included in the genera Corynebacterium, Dermabacter and Brevibacterium. Notably, a specific compound was consistently detected in mycolic acid containing species of the genus Corynebacterium. This compound was composed by glycerol and mycolic acids and structural analyses carried out by fast atom bombardment mass spectrometry in C. minutissimum confirmed its identification as mycoloylglycerol. The chain length of mycoloyl groups in this molecule ranged from 28 to 34 carbon atoms, being mono-, di- or triunsaturated. Detection of mycoloylglycerol by thin-layer chromatography may be thus useful for the rapid inclusion of a great variety of corynebacteria of clinical origin in the genus Corynebacterium in laboratories employing chromatographic techniques as an adjunct for the identification of these microorganisms.

Bacterial Cell Wall Precursor Phosphatase Assays Using Thin-layer Chromatography (TLC) and High Pressure Liquid Chromatography (HPLC)

PubMed Central

Pazos, Manuel; Otten, Christian; Vollmer, Waldemar

2018-01-01

Peptidoglycan encases the bacterial cytoplasmic membrane to protect the cell from lysis due to the turgor. The final steps of peptidoglycan synthesis require a membrane-anchored substrate called lipid II, in which the peptidoglycan subunit is linked to the carrier lipid undecaprenol via a pyrophosphate moiety. Lipid II is the target of glycopeptide antibiotics and several antimicrobial peptides, and is degraded by ‘attacking’ enzymes involved in bacterial competition to induce lysis. Here we describe two protocols using thin-layer chromatography (TLC) and high pressure liquid chromatography (HPLC), respectively, to assay the digestion of lipid II by phosphatases such as Colicin M or the LXG toxin protein TelC from Streptococcus intermedius. The TLC method can also monitor the digestion of undecaprenyl (pyro)phosphate, whereas the HPLC method allows to separate the di-, mono- or unphosphorylated disaccharide pentapeptide products of lipid II. PMID:29651453

A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations

PubMed Central

Badr, Jihan M.

2013-01-01

Background: Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. Materials and Method: In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Results: Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80–1000 ng/spot with respect to the area and correlation coefficient (R2) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5–1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. Conclusion: We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated. PMID:23661986

A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations.

PubMed

Badr, Jihan M

2013-01-01

Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80-1000 ng/spot with respect to the area and correlation coefficient (R(2)) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5-1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated.

Pressurized planar electrochromatography, high-performance thin-layer chromatography and high-performance liquid chromatography--comparison of performance.

PubMed

Płocharz, Paweł; Klimek-Turek, Anna; Dzido, Tadeusz H

2010-07-16

Kinetic performance, measured by plate height, of High-Performance Thin-Layer Chromatography (HPTLC), High-Performance Liquid Chromatography (HPLC) and Pressurized Planar Electrochromatography (PPEC) was compared for the systems with adsorbent of the HPTLC RP18W plate from Merck as the stationary phase and the mobile phase composed of acetonitrile and buffer solution. The HPLC column was packed with the adsorbent, which was scrapped from the chromatographic plate mentioned. An additional HPLC column was also packed with adsorbent of 5 microm particle diameter, C18 type silica based (LiChrosorb RP-18 from Merck). The dependence of plate height of both HPLC and PPEC separating systems on flow velocity of the mobile phase and on migration distance of the mobile phase in TLC system was presented applying test solute (prednisolone succinate). The highest performance, amongst systems investigated, was obtained for the PPEC system. The separation efficiency of the systems investigated in the paper was additionally confirmed by the separation of test component mixture composed of six hormones. 2010 Elsevier B.V. All rights reserved.

Quantitative Determination of Photosynthetic Pigments in Green Beans Using Thin-Layer Chromatography and a Flatbed Scanner as Densitometer

ERIC Educational Resources Information Center

Valverde, Juan; This, Herve; Vignolle, Marc

2007-01-01

A simple method for the quantitative determination of photosynthetic pigments extracted from green beans using thin-layer chromatography is proposed. Various extraction methods are compared, and it is shown how a simple flatbed scanner and free software for image processing can give a quantitative determination of pigments. (Contains 5 figures.)

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

NASA Astrophysics Data System (ADS)

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.

Approximate transient and long time limit solutions for the band broadening induced by the thin sidewall-layer in liquid chromatography columns.

PubMed

Broeckhoven, Ken; Desmet, Gert

2007-11-16

Using a combination of both analytical and numerical techniques, approximate analytical expressions have been established for the transient and long time limit band broadening, originating from the presence of a thin disturbed sidewall layer in liquid chromatography columns, including packed, monolithic as well as microfabricated columns. The established expressions can be used to compare the importance of a thin disturbed sidewall layer with that of other radial heterogeneity effects (such as transcolumn packing density variations due to the relief of packing stresses). The expressions are independent of the actual velocity profile inside the layer as long as the disturbed sidewall layer occupies less than 2.5% of the column width.

Extraction of nutraceuticals from Spirulina (blue-green alga): A bioorganic chemistry practice using thin-layer chromatography.

PubMed

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 current research, theory, and practice, and always in accordance with pedagogical ideas. © 2015 The International Union of Biochemistry and Molecular Biology.

Comparison and characterization of soybean and sunflower lecithins used for chocolate production by high-performance thin-layer chromatography with fluorescence detection and electrospray mass spectrometry.

PubMed

Krüger, Stephanie; Bürmann, Laura; Morlock, Gertrud E

2015-03-25

The scarce availability of nongenetically modified soybeans on the world market represents a growing problem for food manufacturers. Hence, in this study the effects of substituting soybean with sunflower lecithin were investigated with regard to chocolate production. The glycerophospholipid pattern of the different lecithin samples was investigated by high-performance thin-layer chromatography fluorescence detection (HPTLC-FLD) and by HPTLC-positive ion electrospray ionization mass spectrometry (ESI(+)-MS) via the TLC-MS Interface and by scanning HPTLC-matrix-assisted laser desorption ionization-time-of-flight mass spectrometry (MALDI-TOFMS). Especially, the contents of phosphatidylcholine (PC) and phosphatidylethanolamine (PE) were of interest due to the influencing effects of these two glycerophospholipids on the rheological parameters of chocolate production. The lecithin substitution led to only slight differences in the rheological parameters of milk and dark chocolate. Limits of detection (LODs) and limits of quantification (LOQs) of seven glycerophospholipids were studied for three detection modes. Mean LODs ranged from 8 to 40 mg/kg for HPTLC-FLD and, using a single-quadrupole MS, from 10 to 280 mg/kg for HPTLC-ESI(+)-MS as well as from 15 to 310 mg/kg for HPTLC-FLD-ESI(+)-MS recorded after derivatization with the primuline reagent.

Effect-directed fingerprints of 77 botanical extracts via a generic high-performance thin-layer chromatography method combined with assays and mass spectrometry.

PubMed

Krüger, S; Hüsken, L; Fornasari, R; Scainelli, I; Morlock, G E

2017-12-22

Quantitative effect-directed profiles of 77 industrially and freshly extracted botanicals like herbs, spices, vegetables and fruits, widely used as food ingredients, dietary supplements or traditional medicine, gave relevant information on their quality. It allows the assessment of food, dietary supplements and phytomedicines with regard to potential health-promoting activities. In contrary to sum parameter assays and targeted analysis, chromatography combined with effect-directed analysis allows fast assignment of single active compounds and evaluation of their contribution to the overall activity, originating from a food or botanical sample. High-performance thin-layer chromatography was hyphenated with UV/Vis/FLD detection and effect-directed analysis, using the 2,2-diphenyl-1-picrylhydrazyl radical, Gram-negative Aliivibrio fischeri, Gram-positive Bacillus subtilis, acetylcholinesterase and tyrosinase assays. Bioactive compounds of interest were eluted using an elution head-based interface and further characterized by electrospray ionization (high-resolution) mass spectrometry. This highly streamlined workflow resulted in a hyphenated HPTLC-UV/Vis/FLD-EDA-ESI + /ESI - -(HR)MS method. The excellent quantification power of the method was shown on three compounds. For rosmarinic acid, contents ranged from 4.5mg/g (rooibos) to 32.6mg/g (rosemary), for kaempferol-3-glucoside from 0.6mg/g (caraway) to 4.4mg/g (wine leaves), and for quercetin-3-glucoside from 1.1mg/g (hawthorn leaves) to 17.7mg/g (thyme). Three mean repeatabilities (%RSD) over 18 quantifications for the three compounds were ≤2.2% and the mean intermediate precision over three different days (%RSD, n=3) was 5.2%. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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.

Building blocks for the development of an interface for high-throughput thin layer chromatography/ambient mass spectrometric analysis: a green methodology.

PubMed

Cheng, Sy-Chyi; Huang, Min-Zong; Wu, Li-Chieh; Chou, Chih-Chiang; Cheng, Chu-Nian; Jhang, Siou-Sian; Shiea, Jentaie

2012-07-17

Interfacing thin layer chromatography (TLC) with ambient mass spectrometry (AMS) has been an important area of analytical chemistry because of its capability to rapidly separate and characterize the chemical compounds. In this study, we have developed a high-throughput TLC-AMS system using building blocks to deal, deliver, and collect the TLC plate through an electrospray-assisted laser desorption ionization (ELDI) source. This is the first demonstration of the use of building blocks to construct and test the TLC-MS interfacing system. With the advantages of being readily available, cheap, reusable, and extremely easy to modify without consuming any material or reagent, the use of building blocks to develop the TLC-AMS interface is undoubtedly a green methodology. The TLC plate delivery system consists of a storage box, plate dealing component, conveyer, light sensor, and plate collecting box. During a TLC-AMS analysis, the TLC plate was sent to the conveyer from a stack of TLC plates placed in the storage box. As the TLC plate passed through the ELDI source, the chemical compounds separated on the plate would be desorbed by laser desorption and subsequently postionized by electrospray ionization. The samples, including a mixture of synthetic dyes and extracts of pharmaceutical drugs, were analyzed to demonstrate the capability of this TLC-ELDI/MS system for high-throughput analysis.

Characterization of E 471 food emulsifiers by high-performance thin-layer chromatography-fluorescence detection.

PubMed

Oellig, Claudia; Brändle, Klara; Schwack, Wolfgang

2018-07-13

Mono- and diacylglycerol (MAG and DAG) emulsifiers, also known as food additive E 471, are widely used to adjust techno-functional properties in various foods. Besides MAGs and DAGs, E 471 emulsifiers additionally comprise different amounts of triacylglycerols (TAGs) and free fatty acids (FFAs). MAGs, DAGs, TAGs and FFAs are generally determined by high-performance liquid chromatography (HPLC) or gas chromatography (GC) coupled to mass selective detection, analyzing the individual representatives of the lipid classes. In this work we present a rapid and sensitive method for the determination of MAGs, DAGs, TAGs and FFAs in E 471 emulsifiers by high-performance thin-layer chromatography with fluorescence detection (HPTLC-FLD), including a response factor system for quantitation. Samples were simply dissolved and diluted with t-butyl methyl ether before a two-fold development was performed on primuline pre-impregnated LiChrospher silica gel plates with diethyl ether and n-pentane/n-hexane/diethyl ether (52:20:28, v/v/v) as the mobile phases to 18 and 75 mm, respectively. For quantitation, the plate was scanned in the fluorescence mode at UV 366/>400 nm, when the cumulative signal for each lipid class was used. Calibration was done with 1,2-distearin and amounts of lipid classes were calculated with response factors and expressed as monostearin, distearin, tristearin and stearic acid. Limits of detection and quantitation were 1 and 4 ng/zone, respectively, for 1,2-distearin. Thus, the HPTLC-FLD approach represents a simple, rapid and convenient screening alternative to HPLC and GC analysis of the individual compounds. Visual detection additionally enables an easy characterization and the direct comparison of emulsifiers through the lipid class pattern, when utilized as a fingerprint. Copyright © 2018 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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.

In situ Silver Spot Preparation and on-Plate Surface-Enhanced Raman Scattering Detection in Thin Layer Chromatography Separation

NASA Astrophysics Data System (ADS)

Herman, K.; Mircescu, N. E.; Szabo, L.; Leopold, L. F.; Chiş, V.; Leopold, N.

2013-05-01

An improved approach for surface-enhanced Raman scattering (SERS) detection of mixture constituents after thin layer chromatography (TLC) separation is presented. A SERS active silver substrate was prepared under open air conditions, directly on the thin silica film by photo-reduction of silver nitrate, allowing the detection of binary mixtures of cresyl violet, bixine, crystal violet, and Cu(II) complex of 4-(2-pyridylazo)resorcinol. The recorded SERS spectrum provides a unique spectral fingerprint for each molecule; therefore the use of analyte standards is avoided, thus rendering the presented procedure advantageous compared to the conventional detection methodology in TLC.

Digitally enhanced thin layer chromatography: further development and some applications in isotopic chemistry.

PubMed

Manthorpe, Daniel P; Lockley, William J S

2013-09-01

Improvements to thin layer chromatography (TLC) analysis can be made easily and cheaply by the application of digital colour photography and image analysis. The combined technique, digitally enhanced TLC (DE-TLC), is applicable to the accurate quantification of analytes in mixtures, to reaction monitoring and to other typical uses of TLC. Examples are given of the application of digitally enhanced TLC to: the deuteromethylations of theophylline to [methyl-(2)H3]caffeine and of umbelliferone to [(2)H3]7-methoxycoumarin; the selection of tertiary amine bases in deuterodechlorination reactions; stoichiometry optimisation in the borodeuteride reduction of quinizarin (1,4-dihydroxyanthraquinone) and to the assessment of xanthophyll yields in Lepidium sativum seedlings grown in deuterated media. Copyright © 2013 John Wiley & Sons, Ltd.

Surface enhanced Raman scattering imaging of developed thin-layer chromatography plates.

PubMed

Freye, Chris E; Crane, Nichole A; Kirchner, Teresa B; Sepaniak, Michael J

2013-04-16

A method for hyphenating surface enhanced Raman scattering (SERS) and thin-layer chromatography (TLC) is presented that employs silver-polymer nanocomposites as an interface. Through the process of conformal blotting, analytes are transferred from TLC plates to nanocomposite films before being imaged via SERS. A procedure leading to maximum blotting efficiency was established by investigating various parameters such as time, pressure, and type and amount of blotting solvent. Additionally, limits of detection were established for test analytes malachite green isothiocyanate, 4-aminothiophenol, and Rhodamine 6G (Rh6G) ranging from 10(-7) to 10(-6) M. Band broadening due to blotting was minimal (∼10%) as examined by comparing the spatial extent of TLC-spotted Rh6G via fluorescence and then the SERS-based spot size on the nanocomposite after the blotting process. Finally, a separation of the test analytes was carried out on a TLC plate followed by blotting and the acquisition of distance × wavenumber × intensity three-dimensional TLC-SERS plots.

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

PubMed

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

2017-12-01

Quantitative standardization of plant-based products is challenging albeit essential to maintain their quality. 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. 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 F 254 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. The developed method was robust and resolved Ru, Qu, and Ga at R f 0.08 ± 0.02, 0.76 ± 0.01, and 0.63 ± 0.02, respectively. The intra-day, interday precision, and interanalyst were <2% relative standard deviation. The limit of detection and limit of quantification for Ru, Qu, and Ga were 4.51, 4.2, 5.27, and 13.67, 12.73, 15.98 ng/spot, respectively. Antioxidant activity (Log 50% inhibition) of PG and AM was 4.947 ± 0.322 and 6.498 ± 0.295, respectively. The developed HPTLC method was rapid, accurate, precise, reproducible, and specific for the simultaneous estimation of Ru, Qu, and Ga. HPTLC method for simultaneous determination and quantification of Rutin, Quercetin and Gallic acid, is reported for quality control of herbal drugs. Abbreviations Used: A: Aqueous fraction; AM: Aegle marmelos L. Correa; B: Butanol fraction; C: Chloroform fraction; EA: Ethyl acetate fraction; Ga: Gallic acid; H: Hexane fraction; HA: Hydroalcoholic extract; HPTLC: High-performance thin-layer chromatography; PG: Psidium guajava ; Qu: Quercetin; Ru: Rutin.

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

USDA-ARS?s Scientific Manuscript database

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...

The determination and quantification of photosynthetic pigments by reverse phase high-performance liquid chromatography, thin-layer chromatography, and spectrophotometry.

PubMed

Pocock, Tessa; Król, Marianna; Huner, Norman P A

2004-01-01

Chorophylls and carotenoids are functionally important pigment molecules in photosynthetic organisms. Methods for the determination of chlorophylls a and b, beta-carotene, neoxanthin, and the pigments that are involved in photoprotective cycles such as the xanthophylls are discussed. These cycles involve the reversible de-epoxidation of violaxanthin into antheraxanthin and zeaxanthin, as well as the reversible de-epoxidation of lutein-5,6-epoxide into lutein. This chapter describes pigment extraction procedures from higher plants and green algae. Methods for the determination and quantification using high-performance liquid chromatograpy (HPLC) are described as well as methods for the separation and purification of pigments for use as standards using thin-layer chromatography (TLC). In addition, several spectrophotometric methods for the quantification of chlorophylls a and b are described.

Feasibility of correlating separation of ternary mixtures of neutral analytes via thin layer chromatography with supercritical fluid chromatography in support of green flash separations.

PubMed

Ashraf-Khorassani, M; Yan, Q; Akin, A; Riley, F; Aurigemma, C; Taylor, L T

2015-10-30

Method development for normal phase flash liquid chromatography traditionally employs preliminary screening using thin layer chromatography (TLC) with conventional solvents on bare silica. Extension to green flash chromatography via correlation of TLC migration results, with conventional polar/nonpolar liquid mixtures, and packed column supercritical fluid chromatography (SFC) retention times, via gradient elution on bare silica with a suite of carbon dioxide mobile phase modifiers, is reported. Feasibility of TLC/SFC correlation is individually described for eight ternary mixtures for a total of 24 neutral analytes. The experimental criteria for TLC/SFC correlation was assumed to be as follows: SFC/UV/MS retention (tR) increases among each of the three resolved mixture components; while, TLC migration (Rf) decreases among the same resolved mixture components. Successful correlation of TLC to SFC was observed for most of the polar organic solvents tested, with the best results observed via SFC on bare silica with methanol as the CO2 modifier and TLC on bare silica with a methanol/dichloromethane mixture. Copyright © 2015 Elsevier B.V. All rights reserved.

On-chip ultra-thin layer chromatography and surface enhanced Raman spectroscopy.

PubMed

Chen, Jing; Abell, Justin; Huang, Yao-wen; Zhao, Yiping

2012-09-07

We demonstrate that silver nanorod (AgNR) array substrates can be used for on-chip separation and detection of chemical mixtures by combining ultra-thin layer chromatography (UTLC) and surface enhanced Raman spectroscopy (SERS). The UTLC-SERS plate consists of an AgNR array fabricated by oblique angle deposition. The capability of the AgNR substrates to separate the different compounds in a mixture was explored using a mixture of four dyes and a mixture of melamine and Rhodamine 6G at varied concentrations with different mobile phase solvents. After UTLC separation, spatially-resolved SERS spectra were collected along the mobile phase development direction and the intensities of specific SERS peaks from each component were used to generate chromatograms. The AgNR substrates demonstrate the potential for separating the test dyes with plate heights as low as 9.6 μm. The limits of detection are between 10(-5)-10(-6) M. Furthermore, we show that the coupling of UTLC with SERS improves the SERS detection specificity, as small amounts of target analytes can be separated from the interfering background components.

Portable thin layer chromatography for field detection of explosives and propellants

NASA Astrophysics Data System (ADS)

Satcher, Joe H.; Maienschein, Jon L.; Pagoria, Philip F.; Racoveanu, Ana; Carman, M. Leslie; Whipple, Richard E.; Reynolds, John G.

2012-06-01

A field deployable detection kit for explosives and propellants using thin layer chromatography (TLC) has been developed at Lawrence Livermore National Laboratory (LLNL). The chemistry of the kit has been modified to allow for field detection of propellants (through propellant stabilizers), military explosives, peroxide explosives, nitrates and inorganic oxidizer precursors. For many of these target analytes, the detection limit is in the μg to pg range. A new miniaturized, bench prototype, field portable TLC (Micro TLC) kit has also been developed for the detection and identification of common military explosives. It has been demonstrated in a laboratory environment and is ready for field-testing. The kit is comprised of a low cost set of commercially available components specifically assembled for rapid identification needed in the field and identifies the common military explosives: HMX, RDX, Tetryl, Explosive D or picric acid, and TNT all on one plate. Additional modifications of the Micro TLC system have been made with fluorescent organosilicon co-polymer coatings to detect a large suite of explosives.

Thin-Layer and Paper Chromatography.

ERIC Educational Resources Information Center

Sherma, Joseph; Fried, Bernard

1984-01-01

Reviews literature on chromatography examining: books, reviews, student experiments; chromatographic systems, techniques, apparatus; detecting and identification of separated zones; preparative chromatography and radiochromatography; and applications related to specific materials (such as acids, alcohols, amino acids, antibiotics, enzymes, dyes,…

Qualitative and quantitative analysis of hyaluronan oligosaccharides with high performance thin layer chromatography using reagent-free derivatization on amino-modified silica and electrospray ionization-quadrupole time-of-flight mass spectrometry coupling on normal phase.

PubMed

Rothenhöfer, Martin; Scherübl, Rosmarie; Bernhardt, Günther; Heilmann, Jörg; Buschauer, Armin

2012-07-27

Purified oligomers of hyalobiuronic acid are indispensable tools to elucidate the physiological and pathophysiological role of hyaluronan degradation by various hyaluronidase isoenzymes. Therefore, we established and validated a novel sensitive, convenient, rapid, and cost-effective high performance thin layer chromatography (HPTLC) method for the qualitative and quantitative analysis of small saturated hyaluronan oligosaccharides consisting of 2-4 hyalobiuronic acid moieties. The use of amino-modified silica as stationary phase allows a simple reagent-free in situ derivatization by heating, resulting in a very low limit of detection (7-19 pmol per band, depending on the analyzed saturated oligosaccharide). By this derivatization procedure for the first time densitometric quantification of the analytes could be performed by HPTLC. The validated method showed a quantification limit of 37-71 pmol per band and was proven to be superior in comparison to conventional detection of hyaluronan oligosaccharides. The analytes were identified by hyphenation of normal phase planar chromatography to mass spectrometry (TLC-MS) using electrospray ionization. As an alternative to sequential techniques such as high performance liquid chromatography (HPLC) and capillary electrophoresis (CE), the validated HPTLC quantification method can easily be automated and is applicable to the analysis of multiple samples in parallel. Copyright © 2012 Elsevier B.V. All rights reserved.

Application of thin-layer chromatography/infrared matrix-assisted laser desorption/ionization orthogonal time-of-flight mass spectrometry to structural analysis of bacteria-binding glycosphingolipids selected by affinity detection.

PubMed

Müsken, Anne; Souady, Jamal; Dreisewerd, Klaus; Zhang, Wenlan; Distler, Ute; Peter-Katalinić, Jasna; Miller-Podraza, Halina; Karch, Helge; Müthing, Johannes

2010-04-15

Glycosphingolipids (GSLs) play key roles in the manifestation of infectious diseases as attachment sites for pathogens. The thin-layer chromatography (TLC) overlay assay represents one of the most powerful approaches for the detection of GSL receptors of microorganisms. Here we report on the direct structural characterization of microbial GSL receptors by employment of the TLC overlay assay combined with infrared matrix-assisted laser desorption/ionization orthogonal time-of-flight mass spectrometry (IR-MALDI-o-TOF-MS). The procedure includes TLC separation of GSL mixtures, overlay of the chromatogram with GSL-specific bacteria, detection of bound microbes with primary antibodies against bacterial surface proteins and appropriate alkaline phosphatase labeled secondary antibodies, and in situ MS analysis of bacteria-specific GSL receptors. The combined method works on microgram scale of GSL mixtures and is advantageous in that it omits laborious and time-consuming GSL extraction from the silica gel layer. This technique was successfully applied to the compositional analysis of globo-series neutral GSLs recognized by P-fimbriated Escherichia coli bacteria, which were used as model microorganisms for infection of the human urinary tract. Thus, direct TLC/IR-MALDI-o-TOF-MS adds a novel facet to this fast and sensitive method offering a wide range of applications for the investigation of carbohydrate-specific pathogens involved in human infectious diseases. 2010 John Wiley & Sons, Ltd.

Flowing atmospheric pressure afterglow combined with laser ablation for direct analysis of compounds separated by thin-layer chromatography.

PubMed

Cegłowski, Michał; Smoluch, Marek; Reszke, Edward; Silberring, Jerzy; Schroeder, Grzegorz

2016-01-01

A thin-layer chromatography-mass spectrometry (TLC-MS) setup for characterization of low molecular weight compounds separated on standard TLC plates has been constructed. This new approach successfully combines TLC separation, laser ablation, and ionization using flowing atmospheric pressure afterglow (FAPA) source. For the laser ablation, a low-priced 445-nm continuous-wave diode laser pointer, with a power of 1 W, was used. The combination of the simple, low-budget laser pointer and the FAPA ion source has made this experimental arrangement broadly available, also for small laboratories. The approach was successfully applied for the characterization of low molecular weight compounds separated on TLC plates, such as a mixture of pyrazole derivatives, alkaloids (nicotine and sparteine), and an extract from a drug tablet consisting of paracetamol, propyphenazone, and caffeine. The laser pointer used was capable of ablating organic compounds without the need of application of any additional substances (matrices, staining, etc.) on the TLC spots. The detection limit of the proposed method was estimated to be 35 ng/cm(2) of a pyrazole derivative.

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

PubMed

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.

[Analysis of phthalates in plastic food-packaging bags by thin layer chromatography].

PubMed

Chen, Hui; Wang, Yuan; Zhu, Ruohua

2006-01-01

The method for simultaneous determination of four phthalates, namely dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP) and di (2-ethylhexyl) phthalate (DEHP) in plastic food-packaging bags by thin layer chromatography (TLC) was developed. The plastic food-packaging bags were extracted with ethanol by ultrasonication, then the mixture was filtrated through membrane (0.45 microm). The mixture of ethyl acetate-anhydrous ether-isooctane (1 : 4 : 15, v/v) was used as developing agent on the TLC silica gel plate for development. The filtered liquid was spotted on the TLC plate dealt by acetone, and detected with scanning wavelength of 275 nm and reference wavelength of 340 nm. The qualitative analysis of the phthalates was performed using the R(f) values of the chromatogram. The quantitative analysis was performed with external standard method. Good linearities were obtained for DMP, DEP, DBP and DEHP. The detection limits were 2.1 ng for DMP, 2.4 ng for DEP, 3.4 ng for DBP and 4.0 ng for DEHP. The relative standard deviations (RSDs) of the four phthalates were 2.8% - 3.5%. The recoveries of the four phthalate standards in real sample were 78.58% - 111.04%. The method presented has the advantages of high precision, high sensitivity, small sample size, and simple pretreatment . The method was used to detect the four phthalates in the food-packaging bags. The contents in real samples were close to the results by gas chromatography.

Thin-layer chromatography coupled with high performance liquid chromatography for determining tetrabromobisphenol A/S and their derivatives in soils.

PubMed

Liu, Aifeng; Shen, Zhaoshuang; Tian, Yong; Shi, Rongguang; Liu, Yi; Zhao, Zongshan; Xian, Mo

2017-12-01

As brominated flame retardants (BFRs), tetrabromobisphenol A/S (TBBPA/S) and their derivatives have raised wide concerns owing to their widely usage, distributions and adverse effects on human health, thus monitoring these BFRs was urgently needed. In this study, a rapid and cost-effective method based on thin-layer chromatography (TLC) sample pre-treatment coupled with high performance liquid chromatography-diode array detector (HPLC-DAD) (UV=214nm) was developed for determining TBBPA/S and their derivatives in soils, including TBBPA, TBBPA bis(allyl ether) (TBBPA-BAE), TBBPA bis(2,3-dibromopropyl ether) (TBBPA-BDBPE), TBBPS bis(allyl ether) (TBBPS-BAE) and TBBPS bis(2,3-dibromopropyl ether) (TBBPS-BDBPE). The method detection limits (MDLs) and the method quantification limits (MQLs) for these BFRs ranged from 0.023 to 0.087μgg -1 dw and 0.076-0.29μgg -1 dw, respectively. The recoveries were 41-108% and both RSD of repeatability and intermediate precision were less than 11%. The developed method presented good performance for analyzing natural soil samples collected from BFRs industrial park, suggesting its great application potential for monitoring environmental TBBPA/S and their derivatives. Copyright © 2017 Elsevier B.V. All rights reserved.

Chromatography.

ERIC Educational Resources Information Center

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)

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.

PubMed

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.

Analysis of mycolic acids from a group of corynebacteria by capillary gas chromatography and mass spectrometry.

PubMed

Gailly, C; Sandra, P; Verzele, M; Cocito, C

1982-06-15

The cell wall of leprosy-derived corynebacteria (a group of 'diphtheroids' isolated from human leprosy lesions and patients' blood) was previously shown to contain, in addition to peptidoglycan and arabinogalactan, mycolic acids. These alpha-branched beta-hydroxy fatty acids were attributed to the corynomycolic group, according to their RF in monodimensional thin-layer chromatography. In the present work, mycolic acids from leprosy-derived and reference corynebacteria have been fractionated by monodimensional and bidimensional thin-layer chromatography and by gas chromatography. Pyrolyzed mycolic acids have been analyzed on conventional packed columns, whereas intact methyl esters of mycolic acids with free and silylated beta-hydroxyl group have been analyzed on capillary columns, and their structure has been established by mass spectrometry. In all leprosy-derived corynebacteria, some 20 components containing 24-36 carbon atoms and 0-4 double bonds were obtained. The three major groups had 32, 34 and 36 carbons, and the frequency of unsaturated versus saturated chains increased proportionally to the molecular weight. For comparison, the main components of a reference corynebacterium. Corynebacterium diphtheriae PW8, had 30 and 32 carbons, and their hydrocarbon chains were essentially saturated. This work confirms the relative chemical homogeneity of different leprosy-derived corynebacteria and describes some peculiar traits in the chemical structure of this group of organisms. In addition, it shows the complexity of the mycolic acid fraction of corynebacterial cell wall and suggests that the mycolic acid pattern is a sort of fingerprint of each bacterial strain grown under standard conditions. Finally, the fractionation of intact corynomycolic acid methyl esters with free or silylated beta-hydroxyl group by capillary gas chromatography proved to be the best analytical procedure at present available for resolving this complex mixture of corynomycolate isomers

Thin-Layer Chromatography Experiments That Illustrate General Problems in Chromatography.

ERIC Educational Resources Information Center

Lederer, M.; Leipzig-Pagani, E.

1996-01-01

Describes experiments that illustrate a number of general principles such as pattern identification, displacement chromatography, and salting-out adsorption, plus an experiment that demonstrates that identification by chromatography alone is impossible. Illustrates that chromatography is still possible with quite simple means, notwithstanding the…

Secondary metabolite credentials of Evolvulus alsinoides by high performance thin layer chromatography (HPTLC)

PubMed Central

Gomathi, Duraisamy; Kalaiselvi, Manokaran; Ravikumar, Ganesan; Sophia, Dominic; Gopalakrishnan, Velliyur Kanniappan; Uma, Chandrasekar

2012-01-01

Plants and plant-based products are the bases of many modern pharmaceuticals that are current in use today for various diseases. The aim of the study was to investigate the biochemical constituents and high performance thin layer chromatography (HPTLC) finger printing of the ethanolic extract of Evolvulus alsinoides. Phytochemical screening was done by standard procedures and HPTLC method was also established to analyze alkaloids, flavonoids and phenolic compounds from the ethanolic extract of Evolvulus alsinoides. Preliminary phytochemical screening showed that ethanol extracted more secondary metabolites than other solvents. HPTLC fingerprinting analysis showed the presence of various alkaloids, flavonoids and phenols (quercetin) in the ethanolic extract. It can be concluded that Evolvulus alsinoides may serve as a source of potent antioxidants that may be used in the prevention of various diseases such as cancer, diabetes and cardiovascular diseases due to the presence of phenolic compounds. HPTLC finger print of Evolvulus alsinoides may be useful in the differentiation of the species from adulterants and act as a biochemical marker for this medicinally important plant in the pharmaceutical industry and plant systematic studies. PMID:23554763

Quantitative determination of triterpenes from Amphiptherygium adstringens by liquid chromatography and thin-layer chromatography and morphological analysis of cuachalalate preparations.

PubMed

Navarrete, Andres; Avula, Bharathi; Joshi, Vaishali C; Ji, Xiuhong; Hersh, Paul; Khan, Ikhlas A

2006-01-01

Amphiptherygium adstringens (Anacardiaceae/Julianaceae), local name "cuachalalate," is used in folk medicine for the treatment of cholelithiasis, fevers, fresh wounds, hypercholesterolemia, gastritis, gastric ulcers, and cancer of the gastrointestinal tract. The development of column high-performance liquid chromatography-photodiode array detector (LC-PDA) and high-performance thin-layer chromatography (HPTLC)-densitometry methods for the determination of masticadienonic acid and 3-hydroxymasticadienonic acid in cuachalalate preparations is described in this paper. Good separation of the compounds could be achieved by both methods. Either might be preparable depending on the requirements. The LC separation was performed on a Phenomenex Synergi MAX-RP 80A reversed-phase column operated at 40 degrees C with detection at 215 nm. The plant materials were extracted with methanol by sonication. The triterpenes present in the plant material and commercial extracts were separated with an acetonitrile-water reagent alcohol isocratic system. The limit of detection was 0.1-0.2 microg/mL. The relative standard deviation values for the determination of triterpenes in plant extracts were less than 1.00%. This is the first report of an analytical method developed for the quantitative analysis of triterpenes from Amphiptherygium adstringens by LC-PDA and HPTLC. The stem bark showed higher amounts of triterpenes, and low amounts in root and stem root. The microscopic description of the crude drug of cuachalalate was also provided.

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

ERIC Educational Resources Information Center

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)

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

PubMed

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.

The reciprocal iso-inhibition volume concept: A procedure for the evaluation in effect-directed analysis with thin-layer chromatography - using the thin-layer chromatography-luminescent bacteria assay as an example.

PubMed

Schulz, Wolfgang; Weiss, Stefan C; Weber, Walter H; Winzenbacher, Rudi

2017-10-13

In effect-directed analysis (EDA) with high-performance thin-layer chromatography (HPTLC), the effect is often detected using images. Thus, an approach to create inhibition chromatograms from these images was developed using the example of the HPTLC- bioluminescence inhibition test. A comparison between the cuvette test and the HPTLC test shows that the test on the plate is significantly more sensitive. To describe the strength of the effect, the EC 50 value is determined from the dose-response relationship. However, the inhibiting compounds are generally unknown and thus their concentrations are also unknown. Therefore, instead of the concentration, the known application volumes are used. This enables the calculation of the application volume necessary to achieve 50% inhibition. Since the volume is inversely proportional to the concentration, the reciprocal value of the calculated volume is indicated and is referred to as the reciprocal iso-inhibition volume (RIV). Using this RIV-concept, it is now possible to compare inhibition bands within and between plates. The entire evaluation is described by the means of two samples from a contaminated site using the bioluminescence inhibition. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of the Mass Absorption Coefficient in Two-Layer Ti/V and V/Ti Thin Film Systems by the X-Ray Fluorescence Method

NASA Astrophysics Data System (ADS)

Mashin, N. I.; Chernyaeva, E. A.; Tumanova, A. N.; Gafarova, L. M.

2016-03-01

A new XRF procedure for the determination of the mass absorption coefficient in thin film Ti/V and V/Ti two-layer systems has been proposed. The procedure uses easy-to-make thin-film layers of sputtered titanium and vanadium on a polymer film substrate. Correction coefficients have been calculated that take into account attenuation of primary radiation of the X-ray tube, as well as attenuation of the spectral line of the bottom layer element in the top layer.

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

PubMed Central

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

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

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

Yinfa, Ma.

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 bemore » 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.« less

Development of validated high-performance thin layer chromatography for quantification of aristolochic acid in different species of the Aristolochiaceae family.

PubMed

Agrawal, Poonam; Laddha, Kirti

2017-04-01

This study was undertaken to isolate and quantify aristolochic acid in Aristolochia indica stem and Apama siliquosa root. Aristolochic acid is an important biomarker component present in the Aristolochiaceae family. The isolation method involved simple solvent extraction, precipitation and further purification, using recrystallization. The structure of the compound was confirmed using infrared spectroscopy, mass spectrometry and nuclear magnetic resonance. A specific and rapid high-performance thin layer chromatography (HPTLC) method was developed for analysis of aristolochic acid. The method involved separation on the silica gel 60 F 254 plates using the single solvent system of n-hexane: chloroform: methanol. The method showed good linear relationship in the range 0.4-2.0 μg/spot with r 2  = 0.998. The limit of detection and limit of quantification were 62.841 ng/spot and 209.47 ng/spot, respectively. The proposed validated HPTLC method was found to be an easy to use, accurate and convenient method that could be successfully used for standardization and quality assessment of herbal material as well as formulations containing different species of the Aristolochiaceae family. Copyright © 2016. Published by Elsevier B.V.

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

Code of Federal Regulations, 2011 CFR

2011-04-01

... a mixture. The mixture of compounds is absorbed onto a stationary phase or thin layer of inert material (e.g., cellulose, alumina, etc.) and eluted off by a moving solvent (moving phase) until equilibrium occurs between the two phases. (b) Classification. Class I (general controls). The device is...

Arabidopsis thaliana Polar Glycerolipid Profiling by Thin Layer Chromatography (TLC) Coupled with Gas-Liquid Chromatography (GLC)

PubMed Central

Wang, Zhen; Benning, Christoph

2011-01-01

Biological membranes separate cells from the environment. From a single cell to multicellular plants and animals, glycerolipids, such as phosphatidylcholine or phosphatidylethanolamine, form bilayer membranes which act as both boundaries and interfaces for chemical exchange between cells and their surroundings. Unlike animals, plant cells have a special organelle for photosynthesis, the chloroplast. The intricate membrane system of the chloroplast contains unique glycerolipids, namely glycolipids lacking phosphorus: monogalactosyldiacylglycerol (MGDG), digalactosyldiacylglycerol (DGDG), sulfoquinovosyldiacylglycerol (SQDG)4. The roles of these lipids are beyond simply structural. These glycolipids and other glycerolipids were found in the crystal structures of photosystem I and II indicating the involvement of glycerolipids in photosynthesis8,11. During phosphate starvation, DGDG is transferred to extraplastidic membranes to compensate the loss of phospholipids9,12. Much of our knowledge of the biosynthesis and function of these lipids has been derived from a combination of genetic and biochemical studies with Arabidopsis thaliana14. During these studies, a simple procedure for the analysis of polar lipids has been essential for the screening and analysis of lipid mutants and will be outlined in detail. A leaf lipid extract is first separated by thin layer chromatography (TLC) and glycerolipids are stained reversibly with iodine vapor. The individual lipids are scraped from the TLC plate and converted to fatty acyl methylesters (FAMEs), which are analyzed by gas-liquid chromatography coupled with flame ionization detection (FID-GLC) (Figure 1). This method has been proven to be a reliable tool for mutant screening. For example, the tgd1,2,3,4 endoplasmic reticulum-to-plastid lipid trafficking mutants were discovered based on the accumulation of an abnormal galactoglycerolipid: trigalactosyldiacylglycerol (TGDG) and a decrease in the relative amount of 18:3 (carbons

Office Chromatography: Precise printing of sample solutions on miniaturized thin-layer phases and utilization for scanning Direct Analysis in Real Time mass spectrometry.

PubMed

Häbe, Tim T; Morlock, Gertrud E

2015-09-25

Office Chromatography combines achievements in office technologies with miniaturized planar chromatography. In the life sciences, printing of materials became an accepted technique, whereas in separation science, the use of printers for chromatography is at its infancy. A bubble-jet printer was modified for exact application on miniaturized plates. Technical modifications included the removal of all unnecessary parts and the improvement of the positioning system, purge unit and sample supply system. Evaluation was performed via a slide scanner and image evaluation software. Printing of a food dye mixture solution (n=5) led to a calculated mean deposition volume of 13±1nL/mm(2) per print-cycle. A mean determination coefficient (R(2); n=5) of 0.9990 was obtained for application of increasing volumes, executed via increasing band widths of 50-200μm (corresponding to 2-8nL). Using larger band widths and multiple print jobs, deposition volumes of up to the microliter scale represented an alternative to cost-intensive standard equipment. After print, separation, detection and digital evaluation of five food dyes, mean R(2) (n=5) were obtained between 0.9977 and 0.9995. The accuracy of printing was proven by mean recovery rates of 101-105% with repeatabilities of 3-7% (%RSD, n=5). The transfer to nanostructured ultrathin-layer plates proved the synergetic potential of these fields of research. First, this modified printer was suited for printing of finely graduated scales of three preservatives for determination of the spatial resolution of scanning Direct Analysis in Real Time mass spectrometry. Copyright © 2015 Elsevier B.V. All rights reserved.

On the gravitational potential and field anomalies due to thin mass layers

NASA Technical Reports Server (NTRS)

Ockendon, J. R.; Turcotte, D. L.

1977-01-01

The gravitational potential and field anomalies for thin mass layers are derived using the technique of matched asymptotic expansions. An inner solution is obtained using an expansion in powers of the thickness and it is shown that the outer solution is given by a surface distribution of mass sources and dipoles. Coefficients are evaluated by matching the inner expansion of the outer solution with the outer expansion of the inner solution. The leading term in the inner expansion for the normal gravitational field gives the Bouguer formula. The leading term in the expansion for the gravitational potential gives an expression for the perturbation to the geoid. The predictions given by this term are compared with measurements by satellite altimetry. The second-order terms in the expansion for the gravitational field are required to predict the gravity anomaly at a continental margin. The results are compared with observations.

High performance liquid chromatography: Tandem mass spectrometric determination of cisplatin levels in different visceral pleura layers of rats.

PubMed

Xia, Hui; Zhang, Wen; Li, Yingjie; Yu, Changhai

2015-05-01

The aim of the present study was to investigate the concentration of cisplatin in different layers of the visceral pleura in rats, following drug administration. In this study, a sensitive and specific liquid chromatography method coupled with electrospray ionization-tandem mass spectrometry was established to investigate the disposition of cisplatin in different layers of the visceral pleura in rats. Methodological data, including specificity, linearity, accuracy, recovery, precision and lower limits of quantification, confirmed that this novel method may be used to efficiently quantify the cisplatin concentrations in visceral pleura of rats following administration of the drug. Furthermore, the results demonstrated that the desired drug concentration was not achieved in the outer or inner elastic layers of the visceral pleura following injection with cisplatin through various administration methods.

Programmable Electrochemical Rectifier Based on a Thin-Layer Cell.

PubMed

Park, Seungjin; Park, Jun Hui; Hwang, Seongpil; Kwak, Juhyoun

2017-06-21

A programmable electrochemical rectifier based on thin-layer electrochemistry is described here. Both the rectification ratio and the response time of the device are programmable by controlling the gap distance of the thin-layer electrochemical cell, which is easily controlled using commercially available beads. One of the electrodes was modified using a ferrocene-terminated self-assembled monolayer to offer unidirectional charge transfers via soluble redox species. The thin-layer configuration provided enhanced mass transport, which was determined by the gap thickness. The device with the smallest gap thickness (∼4 μm) showed an unprecedented, high rectification ratio (up to 160) with a fast response time in a two-terminal configuration using conventional electronics.

Quantitative thin layer chromatographic multi-sulfonamide screening procedure.

PubMed

Thomas, M H; Soroka, K E; Thomas, S H

1983-07-01

In-situ optical scanning of fluorescamine derivatives on thin layer silica gel plates provides a rapid method for the determination of multiple sulfonamides at levels below 0.1 ppm. Sample preparation is minimal. Homogenized liver or muscle is extracted with ethyl acetate and then back-extracted into 0.2M glycine buffer. After pH adjustment, the extract is washed with hexane and extracted with methylene chloride. The organic phase is evaporated to dryness and reconstituted in methanol. Pre-adsorbent layer silica gel plates are used for chromatography. The method has been applied to residues of sulfamethazine, sulfadimethoxine, sulfathiazole, sulfaquinoxaline, and sulfabromomethazine in cattle, swine, turkey, and duck tissues.

Effect-directed analysis of ginger (Zingiber officinale) and its food products, and quantification of bioactive compounds via high-performance thin-layer chromatography and mass spectrometry.

PubMed

Krüger, S; Bergin, A; Morlock, G E

2018-03-15

Decision makers responsible for quality management along the food chain need to reflect on their analytical tools that should ensure quality of food and especially superfood. The "4ables" in target analysis (stable, extractable, separable, detectable) focusing on marker compounds do not cover all relevant information about the sample. On the example of ginger, a streamlined quantitative bioprofiling was developed for effect-directed analysis of 17 commercially available ginger and ginger-containing products via high-performance thin-layer chromatography (HPTLC-UV/Vis/FLD-bioassay). The samples were investigated concerning their active profile as radical scavengers, antimicrobials, estrogen-like activators and acetylcholinesterase/tyrosinase inhibitors. The [6]-gingerol and [6]-shogaol content of the different products ranged 0.2-7.4mg/g and 0.2-3.0mg/g, respectively. Further, multipotent compounds were discovered, characterized, and for example, assigned as [8]- and [10]-gingerol via HPTLC-ESI-HRMS. The developed bioprofiling is a step forward to new analytical methods needed to inform on the true product quality influenced by cultivation, processing, and storage. Copyright © 2017 Elsevier Ltd. All rights reserved.

A simple liquid extraction protocol for overcoming the ion suppression of triacylglycerols by phospholipids in liquid chromatography mass spectrometry studies.

PubMed

Araujo, Pedro; Tilahun, Ephrem; Breivik, Joar Fjørtoft; Abdulkader, Bashir M; Frøyland, Livar; Zeng, Yingxu

2016-02-01

It is well-known that triacylglycerol (TAG) ions are suppressed by phospholipid (PL) ions in regiospecific analysis of TAG by mass spectrometry (MS). Hence, it is essential to remove the PL during sample preparation prior to MS analysis. The present article proposes a cost-effective liquid-liquid extraction (LLE) method to remove PL from TAG in different kinds of biological samples by using methanol, hexane and water. High performance thin layer chromatography confirmed the lack of PL in krill oil and salmon liver samples, submitted to the proposed LLE protocol, and liquid chromatography tandem MS confirmed that the identified TAG ions were highly enhanced after implementing the LLE procedure. Copyright © 2015 Elsevier B.V. All rights reserved.

Highly sensitive on-site detection of drugs adulterated in botanical dietary supplements using thin layer chromatography combined with dynamic surface enhanced Raman spectroscopy.

PubMed

Fang, Fang; Qi, Yunpeng; Lu, Feng; Yang, Liangbao

2016-01-01

The phenomenon of botanical dietary supplements (BDS) doped with illegal adulterants has become a serious problem all over the world, which could cause great threat to human's health. Therefore, it is of great value to identify BDS. Herein, we put forward a highly sensitive method for on-site detection of antitussive and antiasthmatic drugs adulterated in BDS using thin layer chromatography (TLC) combined with dynamic surface enhanced Raman spectroscopy (DSERS). Adulterants in BDS were separated on a TLC plate and located under UV illumination. Then DSERS detection was performed using a portable Raman spectrometer with 50% glycerol silver colloid serving as DSERS active substrate. Here, the effects of different solvents on detection efficacy were evaluated using phenformin hydrochloride (PHE) as a probe. It was shown that 50% glycerol resulted in higher SERS enhancement and relatively higher stability. Moreover, practical application of this novel TLC-DSERS method was demonstrated with rapid analysis of real BDS samples and one sample adulterated with benproperine phosphate (BEN) was found. Furthermore, the obtained result was verified by ultra performance liquid chromatography-quadrupole time of flight mass spectrometry (UPLC-QTOF/MS). The sensitivity of the TLC-DSERS technique is 1-2 orders of magnitude higher than that of TLC-SERS technique. The results turned out that this combined method would have good prospects for on-site and sensitive detection of adulterated BDS. Copyright © 2015 Elsevier B.V. All rights reserved.

Layer chromatography-bioassays directed screening and identification of antibacterial compounds from Scotch thistle.

PubMed

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.

Lipophilicity Assessment of Ruthenium(II)-Arene Complexes by the Means of Reversed-Phase Thin-Layer Chromatography and DFT Calculations

PubMed Central

Shweshein, Khalil Salem A. M.; Andrić, Filip; Radoičić, Aleksandra; Gruden-Pavlović, Maja; Tešić, Živoslav; Milojković-Opsenica, Dušanka

2014-01-01

The lipophilicity of ten ruthenium(II)-arene complexes was assessed by reversed-phase thin-layer chromatography (RP-TLC) on octadecyl silica stationary phase. The binary solvent systems composed of water and acetonitrile were used as mobile phase in order to determine chromatographic descriptors for lipophilicity estimation. Octanol-water partition coefficient, logK OW, of tested complexes was experimentally determined using twenty-eight standard solutes which were analyzed under the same chromatographic conditions as target substances. In addition, ab initio density functional theory (DFT) computational approach was employed to calculate logK OW values from the differences in Gibbs' free solvation energies of the solute transfer from n-octanol to water. A good overall agreement between DFT calculated and experimentally determined logK OW values was established (R 2 = 0.8024–0.9658). PMID:24587761

Validation Thin Layer Chromatography for the Determination of Acetaminophen in Tablets and Comparison with a Pharmacopeial Method

PubMed Central

Pyka, Alina; Budzisz, Marika; Dołowy, Małgorzata

2013-01-01

Adsorption thin layer chromatography (NP-TLC) with densitometry has been established for the identification and the quantification of acetaminophen in three leading commercial products of pharmaceutical tablets coded as brand: P1 (Product no. 1), P2 (Product no. 2), and P3 (Product no. 3). Applied chromatographic conditions have separated acetaminophen from its related substances, namely, 4-aminophenol and and 4′-chloroacetanilide. UV densitometry was performed in absorbance mode at 248 nm. The presented method was validated by specificity, range, linearity, accuracy, precision, detection limit, quantitative limit, and robustness. The TLC-densitometric method was also compared with a pharmacopeial UV-spectrophotometric method for the assay of acetaminophen, and the results confirmed statistically that the NP-TLC-densitometric method can be used as a substitute method. It could be said that the validated NP-TLC-densitometric method is suitable for the routine analysis of acetaminophen in quantity control laboratories. PMID:24063006

Determination of cortisol in human plasma by thin-layer chromatography and fluorescence derivatization with isonicotinic acid hydrazide.

PubMed

Fenske, Martin

2008-01-01

The present work describes a specific and rapid determination of cortisol in human plasma. The method includes liquid-liquid extraction of plasma samples, thin-layer chromatography (TLC) of ethanolic extracts on aluminium foil-backed silica gel 60 TLC plates, derivatization of cortisol with isonicotinic acid hydrazide, and densitometric measurement of the fluorescence intensity of cortisol hydrazone. The fluorescence was linearly related to cortisol amounts; the correlation coefficients of standard curve plots were r>0.99. The coefficient of variation ranged between 2.8-7.9% (20 ng, within-assay/between assay variation) and 1.6-6.8% (80 ng, within-assay/between assay variation). The recovery of cortisol from plasma spiked with 21-deoxycortisol was 85%+/-4%. Cortisol concentration in the plasma was 66+/-32 ng/mL (mean+/-standard deviation, n=24). The advantage of this method is its simplicity to separate cortisol from other steroids by TLC, its specificity (formation of cortisol hydrazone), and the rapid quantitation of cortisol by densitometry.

Observations of metal concentrations in E-region sporadic thin layers using incoherent-scatter radar

NASA Astrophysics Data System (ADS)

Suzuki, Nobuhiro

This thesis has used incoherent-scatter radar data from the facility at Sondrestrom, Greenland to determine the ion mass values inside thin sporadic-E layers in the lower ionosphere. Metallic positively-charged ions of meteoric origin are deposited in the earth's upper atmosphere over a height range of about 85-120 km. Electric fields and neutral-gas (eg N2, O, O2) winds at high latitudes may produce convergent ion dynamics that results in the re-distribution of the background altitude distribution of the ions to form thin (1-3 km) high-density layers that are detectable with radar. A large database of experimental radar observations has been processed to determine ion mass values inside these thin ion layers. The range resolution of the radar was 600 meters that permitted mass determinations at several altitude steps within the layers. Near the lower edge of the layers the ion mass values were in the range 20-25 amu while at the top portion of the layers the mass values were generally in the range 30-40 amu. The numerical values are consistent with in-situ mass spectrometer data obtained by other researchers that suggest these layers are mainly composed of a mixture or Mg +, Si+, and Fe + ions. The small tendency for heavier ions to reside at the top portion of the layers is consistent with theory. The results have also found new evidence for the existence of complex-shaped multiple layers; the examples studied suggest similar ion mass values in different layers that in some cases are separated in altitude by several km.

Simultaneous Determination of Withanolide A and Bacoside A in Spansules by High-Performance Thin-Layer Chromatography

PubMed Central

Shinde, P B; Aragade, P D; Agrawal, M R; Deokate, U A; Khadabadi, S S

2011-01-01

The objective of this work was to develop and validate a simple, rapid, precise, and accurate high performance thin layer chromatography method for simultaneous determination of withanolide A and bacoside A in combined dosage form. The stationary phase used was silica gel G60F254. The mobile phase used was mixture of ethyl acetate: methanol: toluene: water (4:1:1:0.5 v/v/v/v). The detection of spots was carried out at 320 nm using absorbance reflectance mode. The method was validated in terms of linearity, accuracy, precision and specificity. The calibration curve was found to be linear between 200 to 800 ng/spot for withanolide A and 50 to 350 ng/spot for bacoside A. The limit of detection and limit of quantification for the withanolide A were found to be 3.05 and 10.06 ng/spot, respectively and for bacoside A 8.3 and 27.39 ng/spot, respectively. The proposed method can be successfully used to determine the drug content of marketed formulation. PMID:22303073

Simultaneous determination of withanolide a and bacoside a in spansules by high-performance thin-layer chromatography.

PubMed

Shinde, P B; Aragade, P D; Agrawal, M R; Deokate, U A; Khadabadi, S S

2011-03-01

The objective of this work was to develop and validate a simple, rapid, precise, and accurate high performance thin layer chromatography method for simultaneous determination of withanolide A and bacoside A in combined dosage form. The stationary phase used was silica gel G60F(254). The mobile phase used was mixture of ethyl acetate: methanol: toluene: water (4:1:1:0.5 v/v/v/v). The detection of spots was carried out at 320 nm using absorbance reflectance mode. The method was validated in terms of linearity, accuracy, precision and specificity. The calibration curve was found to be linear between 200 to 800 ng/spot for withanolide A and 50 to 350 ng/spot for bacoside A. The limit of detection and limit of quantification for the withanolide A were found to be 3.05 and 10.06 ng/spot, respectively and for bacoside A 8.3 and 27.39 ng/spot, respectively. The proposed method can be successfully used to determine the drug content of marketed formulation.

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

USDA-ARS?s Scientific Manuscript database

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. fungal spores in nutrient solution or bacteria in liquefied agar), allowing time for the microbes to gr...

Characterization of drug authenticity using thin-layer chromatography imaging with a mobile phone.

PubMed

Yu, Hojeong; Le, Huy M; Kaale, Eliangiringa; Long, Kenneth D; Layloff, Thomas; Lumetta, Steven S; Cunningham, Brian T

2016-06-05

Thin-layer chromatography (TLC) has a myriad of separation applications in chemistry, biology, and pharmacology due to its simplicity and low cost. While benchtop laboratory sample application and detection systems for TLC provide accurate quantitation of TLC spot positions and densities, there are many applications where inexpensive and portable instruments would greatly expand the applicability of the technology. In this work, we demonstrate identity verification and concentration determination of pharmaceutical compounds via TLC using a custom 3D-printed cradle that interfaces with an ordinary mobile phone. The cradle holds the mobile phone's internal, rear-facing camera in a fixed position relative to a UV lamp and a TLC plate that includes a phosphor in the stationary phase. Analysis of photographs thus reveals the locations and intensities of principal spots of UV--absorbing drugs. Automated image analysis software determines the center location and density of dark spots, which, using integrated calibration spots of known drug compounds and concentrations, can be used to determine if a drug has been diluted or substituted. Two independent image processing approaches have been developed that may be selected based upon the processing capabilities of the smartphone. Each approach is able to discern 5% drug concentration differences. Using single-component solutions of nevirapine, amodiaquine, and paracetamol that have been manually applied, the mobile phone-based detection instrument provides measurements that are equivalent to those obtained with a commercially available lab-based desktop TLC densitometer. Copyright © 2016 Elsevier B.V. All rights reserved.

Lysergic acid amide as chemical marker for the total ergot alkaloids in rye flour - Determination by high-performance thin-layer chromatography-fluorescence detection.

PubMed

Oellig, Claudia

2017-07-21

Ergot alkaloids are generally determined by high-performance liquid chromatography (HPLC) coupled to fluorescence detection (FLD) or mass selective detection, analyzing the individual compounds. However, fast and easy screening methods for the determination of the total ergot alkaloid content are more suitable, since for monitoring only the sum of the alkaloids is relevant. The herein presented screening uses lysergic acid amide (LSA) as chemical marker, formed from ergopeptine alkaloids, and ergometrine for the determination of the total ergot alkaloids in rye with high-performance thin-layer chromatography-fluorescence detection (HPTLC-FLD). An ammonium acetate buffered extraction step was followed by liquid-liquid partition for clean-up before the ergopeptine alkaloids were selectively transformed to LSA and analyzed by HPTLC-FLD on silica gel with isopropyl acetate/methanol/water/25% ammonium hydroxide solution (80:10:3.8:1.1, v/v/v/v) as the mobile phase. The enhanced native fluorescence of LSA and unaffected ergometrine was used for quantitation without any interfering matrix. Limits of detection and quantitation were 8 and 26μg LSA/kg rye, which enables the determination of the total ergot alkaloids far below the applied quality criterion limit for rye. Close to 100% recoveries for different rye flours at relevant spiking levels were obtained. Thus, reliable results were guaranteed, and the fast and efficient screening for the total ergot alkaloids in rye offers a rapid alternative to the HPLC analysis of the individual compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

Bioprofiling of Salicaceae bud extracts through high-performance thin-layer chromatography hyphenated to biochemical, microbiological and chemical detections.

PubMed

Hage, Salim; Morlock, Gertrud E

2017-03-24

The buds of poplars (Populus L.) and willows (Salix L.), both from the same family (Salicaceae Mirbel), are increasingly used in gemmotherapy and importantly contribute to the production of the physiologically active propolis by European bee Apis mellifera L. In order to study their phenolic profiles, polar extracts of buds from P. nigra L. were compared to those of P. alba L. and S. alba L. through high-performance thin-layer chromatography (HPTLC). Five chemotypical patterns were distinguished after derivatisation with the Natural Product reagent and confirmed by principal component analysis. The HPTLC analysis was directly hyphenated to various microbiological and biochemical assays as well as spectrometric techniques, directly linking to active molecules in the chromatograms. At a glance, polyvalent compounds were evident when all derivatisation and activity assays, to which HPTLC was hyphenated at ease, were combined together. In Populus buds, at least three antimicrobial compound zones were detected using Aliivibrio fischeri and Bacillus subtilis bioassays, and one phyto-œstrogen with the planar yeast œstrogen screen. In all samples, several inhibitors of acetyl- and butyrylcholinesterase and rabbit liver esterase were detected. Hyphenation to high resolution mass spectrometry supported the assignment of bioactive compounds, as shown for chrysin as selective cholinesterase inhibitor as well as caffeic acid and galangin as antimicrobials in P. nigra and P. alba. This fast and cost-efficient method can be appropriately extended and applied to the botanical origin determination and quality control of bud extracts and propolis samples. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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.

Identification of arsenobetaine in sole, lemon sole, flounder, dab, crab and shrimps by field desorption and fast atom bombardment mass spectrometry

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

Luten, J.B.; Riekwel-Booy, G.; Greef, M.C.

1983-01-01

Organo-arsenic has been isolated from sole, lemon sole, flounder, dab, crab and shrimps by extraction or ion-exchange in combination with thin-layer chromatography. An alkaline digestion of the samples, followed by a reduction with sodiumborohydride leads to the formation of trimethylarsine. Field desorption mass spectrometry (FDMS) can be used to identify arsenobetaine in the isolates. Sufficient purification by thin-layer chromatography is found to be a prerequisite for the detection of a protonated molecular ion of arsenobetaine. If this situation is not met acid enchanced FDMS or Fast Atom Bombardment mass spectrometry in high resolution can be used successfully.

Quantitative Caffeine Analysis Using a Surface Sampling Probe Electrospray Ionization Tandem Mass Spectrometry System

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

Ford, Michael J; Deibel, Michael A.; Tomkins, Bruce A

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 methodsmore » 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.« less

Stripping analysis of nanomolar perchlorate in drinking water with a voltammetric ion-selective electrode based on thin-layer liquid membrane.

PubMed

Kim, Yushin; Amemiya, Shigeru

2008-08-01

A highly sensitive analytical method is required for the assessment of nanomolar perchlorate contamination in drinking water as an emerging environmental problem. We developed the novel approach based on a voltammetric ion-selective electrode to enable the electrochemical detection of "redox-inactive" perchlorate at a nanomolar level without its electrolysis. The perchlorate-selective electrode is based on the submicrometer-thick plasticized poly(vinyl chloride) membrane spin-coated on the poly(3-octylthiophene)-modified gold electrode. The liquid membrane serves as the first thin-layer cell for ion-transfer stripping voltammetry to give low detection limits of 0.2-0.5 nM perchlorate in deionized water, commercial bottled water, and tap water under a rotating electrode configuration. The detection limits are not only much lower than the action limit (approximately 246 nM) set by the U.S. Environmental Protection Agency but also are comparable to the detection limits of the most sensitive analytical methods for detecting perchlorate, that is, ion chromatography coupled with a suppressed conductivity detector (0.55 nM) or electrospray ionization mass spectrometry (0.20-0.25 nM). The mass transfer of perchlorate in the thin-layer liquid membrane and aqueous sample as well as its transfer at the interface between the two phases were studied experimentally and theoretically to achieve the low detection limits. The advantages of ion-transfer stripping voltammetry with a thin-layer liquid membrane against traditional ion-selective potentiometry are demonstrated in terms of a detection limit, a response time, and selectivity.

Separation of pigment formulations by high-performance thin-layer chromatography with automated multiple development.

PubMed

Stiefel, Constanze; Dietzel, Sylvia; Endress, Marc; Morlock, Gertrud E

2016-09-02

Food packaging is designed to provide sufficient protection for the respective filling, legally binding information for the consumers like nutritional facts or filling information, and an attractive appearance to promote the sale. For quality and safety of the package, a regular quality control of the used printing materials is necessary to get consistently good print results, to avoid migration of undesired ink components into the food and to identify potentially faulty ink batches. Analytical approaches, however, have hardly been considered for quality assurance so far due to the lack of robust, suitable methods for the analysis of rarely soluble pigment formulations. Thus, a simple and generic high-performance thin-layer chromatography (HPTLC) method for the separation of different colored pigment formulations was developed on HPTLC plates silica gel 60 by automated multiple development. The gradient system provided a sharp resolution for differently soluble pigment constituents like additives and coating materials. The results of multi-detection allowed a first assignment of the differently detectable bands to particular chemical substance classes (e.g., lipophilic components), enabled the comparison of different commercially available pigment batches and revealed substantial variations in the composition of the batches. Hyphenation of HPTLC with high resolution mass spectrometry and infrared spectroscopy allowed the characterization of single unknown pigment constituents, which may partly be responsible for known quality problems during printing. The newly developed, precise and selective HPTLC method can be used as part of routine quality control for both, incoming pigment batches and monitoring of internal pigment production processes, to secure a consistent pigment composition resulting in consistent ink quality, a faultless print image and safe products. Hyphenation of HPTLC with the A. fischeri bioassay gave first information on the bioactivity or rather

Simultaneous Determination of Size and Quantification of Gold Nanoparticles by Direct Coupling Thin layer Chromatography with Catalyzed Luminol Chemiluminescence

PubMed Central

Yan, Neng; Zhu, Zhenli; He, Dong; Jin, Lanlan; Zheng, Hongtao; Hu, Shenghong

2016-01-01

The increasing use of metal-based nanoparticle products has raised concerns in particular for the aquatic environment and thus the quantification of such nanomaterials released from products should be determined to assess their environmental risks. In this study, a simple, rapid and sensitive method for the determination of size and mass concentration of gold nanoparticles (AuNPs) in aqueous suspension was established by direct coupling of thin layer chromatography (TLC) with catalyzed luminol-H2O2 chemiluminescence (CL) detection. For this purpose, a moving stage was constructed to scan the chemiluminescence signal from TLC separated AuNPs. The proposed TLC-CL method allows the quantification of differently sized AuNPs (13 nm, 41 nm and 100 nm) contained in a mixture. Various experimental parameters affecting the characterization of AuNPs, such as the concentration of H2O2, the concentration and pH of the luminol solution, and the size of the spectrometer aperture were investigated. Under optimal conditions, the detection limits for AuNP size fractions of 13 nm, 41 nm and 100 nm were 38.4 μg L−1, 35.9 μg L−1 and 39.6 μg L−1, with repeatabilities (RSD, n = 7) of 7.3%, 6.9% and 8.1% respectively for 10 mg L−1 samples. The proposed method was successfully applied to the characterization of AuNP size and concentration in aqueous test samples. PMID:27080702

Ultra-thin layer chromatography and surface enhanced Raman spectroscopy on silver nanorod array substrates prepared by oblique angle deposition

NASA Astrophysics Data System (ADS)

Chen, Jing; Abell, Justin; Huang, Yao-wen; Zhao, Yiping

2012-06-01

We demonstrate the potential use of silver nanorod (AgNR) array substrates for on-chip separation and detection of chemical mixtures by ultra-thin layer chromatography (UTLC) and surface enhanced Raman spectroscopy (SERS). The capability of the AgNR substrates to separate different compounds in a mixture was explored using a mixture of the food colorant Brilliant Blue FCF and lactic acid, and the mixtures of Methylene Violet and BSA at various concentrations. After the UTLC process, spatially-resolved SERS spectra were collected along the mobile phase development direction and the intensities of specific SERS peaks from each component were used to generate chromatograms. The AgNR substrates demonstrate the capability of separating Brilliant Blue from lactic acid, as well as revealing the SERS signal of Methylene Violet from the massive BSA background after a simple UTLC step. This technique may have significant practical implications in actual detection of small molecules from complex food or clinical backgrounds.

Improved thin-layer chromatography bioautographic assay for the detection of actylcholinesterase inhibitors in plants.

PubMed

Yang, Zhong-Duo; Song, Zhu-Wen; Ren, Jin; Yang, Ming-Jun; Li, Shuo

2011-01-01

Thin-layer chromatography (TLC) bioautographic method is a simple and rapid method to screen acetylcholinesterase inhibitors from plant extracts. However, the high consumption of enzyme (6 U/mL) in current methods makes the procedure expensive, which is an obstacle to scientific research centers lacking funding. To develop a new low-cost TLC bioautographic method. A series of compounds, as substrates, were synthesised and their ability to be hydrolysed by acetylcholinesterase was evaluated by the HPLC method. 4-Methoxyphenyl acetate (14) was proved to be an appropriate substrate for TLC bioautographic assay. Therefore a new and cheap TLC bioautographic assay was set up. The mechanism of this new method is that the enzyme converts 4-methoxylphenyl acetate into 4-methoxyphenol, which reacts with a solution of potassium ferricyanide ([K₃(FeCN)₆]) and iron chloride hexahydrate (FeCl₃·6H₂O) to make an aquamarine blue coloured background on the TLC plates. Regions of the TLC plate which contain acetylcholinesterase inhibitors show up as light yellow spots against the background. The consumption of enzyme (1 U/mL) in the new method is low and the detection limit of two known acetylcholinesterase inhibitors, huperzine A (0.0001 μg) and physostigmine (0.001 μg), for this assay are close to published values. A low-cost TLC bioautographic method was developed, which will benefit research groups pursuing natural acetylcholinesterase inhibitors. Copyright © 2011 John Wiley & Sons, Ltd.

Method of transferring a thin crystalline semiconductor layer

DOEpatents

Nastasi, Michael A [Sante Fe, NM; Shao, Lin [Los Alamos, NM; Theodore, N David [Mesa, AZ

2006-12-26

A method for transferring a thin semiconductor layer from one substrate to another substrate involves depositing a thin epitaxial monocrystalline semiconductor layer on a substrate having surface contaminants. An interface that includes the contaminants is formed in between the deposited layer and the substrate. Hydrogen atoms are introduced into the structure and allowed to diffuse to the interface. Afterward, the thin semiconductor layer is bonded to a second substrate and the thin layer is separated away at the interface, which results in transferring the thin epitaxial semiconductor layer from one substrate to the other substrate.

Amorphous silicon Schottky barrier solar cells incorporating a thin insulating layer and a thin doped layer

DOEpatents

Carlson, David E.

1980-01-01

Amorphous silicon Schottky barrier solar cells which incorporate a thin insulating layer and a thin doped layer adjacent to the junction forming metal layer exhibit increased open circuit voltages compared to standard rectifying junction metal devices, i.e., Schottky barrier devices, and rectifying junction metal insulating silicon devices, i.e., MIS devices.

Comparison of results for morphine urinalyses by radioimmunoassay and thin-layer chromatography in a narcotic clinic setting.

PubMed

Kokoski, R J; Jain, M

1975-03-01

Radioimmunoassay (RIA) and thin-layer chromatography (TLC) were compared for morphine detection in an actual narcotic clinic setting. A choice of urines from all those screened by TLC allowed a critical comparison as to actual use or non-use of narcotic drugs, rather than a sampling at random in which the question of possible false positives or negatives cannot be conclusively answered. Although RIA is more sensitive than TLC, its advantage is apparent only in those cases where urine specimens are difficult to obtain frequently regularly or where the use of morphine is suspected by the positive identification of quinine in urine that was morphine-negative by TLC. In a selected group of negative and positive specimens chosen without conscious bias, the two methods gave consistently similar results, indicating that the modified TLC method provided a few or no false positives or negatives if the negatives were from those cases that were not positive anytime up to 3-4 days before urine collection. We conclude that RIA can be of significant value as a supplement to a TLC screening program, without sacrificing the many advantages that TLC has to offer.

Separation, identification and quantification of carotenoids and chlorophylls in dietary supplements containing Chlorella vulgaris and Spirulina platensis using High Performance Thin Layer Chromatography.

PubMed

Hynstova, Veronika; Sterbova, Dagmar; Klejdus, Borivoj; Hedbavny, Josef; Huska, Dalibor; Adam, Vojtech

2018-01-30

In this study, 14 commercial products (dietary supplements) containing alga Chlorella vulgaris and cyanobacteria Spirulina platensis, originated from China and Japan, were analysed. UV-vis spectrophotometric method was applied for rapid determination of chlorophylls, carotenoids and pheophytins; as degradation products of chlorophylls. High Performance Thin-Layer Chromatography (HPTLC) was used for effective separation of these compounds, and also Atomic Absorption Spectrometry for determination of heavy metals as indicator of environmental pollution. Based on the results obtained from UV-vis spectrophotometric determination of photosynthetic pigments (chlorophylls and carotenoids), it was confirmed that Chlorella vulgaris contains more of all these pigments compared to the cyanobacteria Spirulina platensis. The fastest mobility compound identified in Chlorella vulgaris and Spirulina platensis using HPTLC method was β-carotene. Spectral analysis and standard calibration curve method were used for identification and quantification of separated substances on Thin-Layer Chromatographic plate. Quantification of copper (Cu 2+ , at 324.7 nm) and zinc (Zn 2+ , at 213.9nm) was performed using Flame Atomic Absorption Spectrometry with air-acetylene flame atomization. Quantification of cadmium (Cd 2+ , at 228.8 nm), nickel (Ni 2+ , at 232.0nm) and lead (Pb 2+ , at 283.3nm) by Electrothermal Graphite Furnace Atomic Absorption Spectrometry; and quantification of mercury (Hg 2+ , at 254nm) by Cold Vapour Atomic Absorption Spectrometry. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed Central

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

2015-01-01

Objective: 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. Materials and Methods: 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. Results: 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. Conclusions: 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. PMID:26681890

Thin-layer chromatographic technique for rapid detection of bacterial phospholipases.

PubMed

Legakis, N J; Papavassiliou, J

1975-11-01

Silica gel thin-layer chromatography was employed to detect lecithinase activity induced from bacterial resting cell preparations induced from bacterial resting cell preparations incubated at 37 C for 4 h in the presence of purified egg yolk lecithin. Bacillus subtilis, Bacillus cereus, Serratia marcescens, and Pseudomonas aeruginosa hydrolyzed lecithin with the formation of free fatty acids as the sole lipid-soluble product. In none of the Escherichia coli and Citrobacter freundii strains tested could lecithinase activity be detected. Four among eight strains of Enterobacter aerogenes and one among 12 strains of Proteus tested produced negligible amounts of free fatty acid.

Phospholipid composition of cell-derived microparticles determined by one-dimensional high-performance thin-layer chromatography.

PubMed

Weerheim, A M; Kolb, A M; Sturk, A; Nieuwland, R

2002-03-15

Microparticles in the circulation activate the coagulation system and may activate the complement system via C-reactive protein upon conversion of membrane phospholipids by phospholipases. We developed a sensitive and reproducible method to determine the phospholipid composition of microparticles. Samples were applied to horizontal, one-dimensional high-performance thin-layer chromatography (HPTLC). Phospholipids were separated on HPTLC by chloroform:ethyl acetate:acetone:isopropanol:ethanol:methanol:water:acetic acid (30:6:6:6:16:28:6:2); visualized by charring with 7.5% Cu-acetate (w/v), 2.5% CuSO(4) (w/v), and 8% H(3)PO(4) (v/v) in water; and quantified by photodensitometric scanning. Erythrocyte membranes were used to validate the HPTLC system. Microparticles were isolated from plasma of healthy individuals (n = 10). On HPTLC, mixtures of (purified) phospholipids, i.e., lysophosphatidylcholine, phosphatidylcholine (PC), sphingomyelin (SM), lysophosphatidylserine, phosphatidylserine, lysophosphatidylethanolamine, phosphatidylethanolamine (PE), and phosphatidylinositol, could be separated and quantified. All phospholipids were detectable in erythrocyte ghosts, and their quantities fell within ranges reported earlier. Quantitation of phospholipids, including extraction, was highly reproducible (CV < 10%). Microparticles contained PC (59%), SM (20.6%), and PE (9.4%), with relatively minor (<5%) quantities of other phospholipids. HPTLC can be used to study the phospholipid composition of cell-derived microparticles and may also be a useful technique for the analysis of other samples that are available only in minor quantities. (C)2002 Elsevier Science (USA).

Re-evaluation of thin layer chromatography as an alternative method for the quantification of prostaglandins from rat Kupffer cells.

PubMed

Pestel, Sabine; Jungermann, Kurt; Schieferdecker, Henrike L

2005-01-01

In contrast to conventionally used immunoassays, thin layer chromatography (TLC)--by prelabeling of cells with radioactive arachidonic acid (AA)--allows to differentiate between cellularly built and added prostanoids and thus to investigate feedback effects of prostanoids on their own release. PGD2, TXB2 and PGE2 released from zymosan-stimulated Kupffer cells were separated with distinct RF-values, corresponding to those of the pure substances. Quantification of PGD2 and PGE2 gave comparable results with TLC and immunoassays, but measurement in the presence of added prostanoids was only possible with TLC. Moreover TLC was superior to immunoassays in having a longer linear range while being comparably sensitive. Cellularly built TXB2 in its radioactively labeled form was not detectable by TLC. Inhibition of TXB2 release by externally added AA or technical artifacts were excluded, suggesting that the cellular AA-pools used for prostaglandin and thromboxane synthesis differ in their accessibility for added AA. Thus, TLC is a simple, sensitive and precise method for the quantification of cellularly built prostaglandins but not of thromboxane even in the presence of added prostanoids.

Variables affecting resolution of lung phospholipids in one-dimensional thin-layer chromatography.

PubMed

Krahn, J

1987-01-01

Resolution of the confusion in the literature about the separation of lung phospholipids in thin-layer chromatographic systems has awaited a systematic study of the variables that potentially affect this separation. In this study I show that: incorporation of ammonium sulfate into silica gel "GHL" has a dramatic effect on separation of lung phospholipids; this effect is equally dramatic but different in activated and nonactivated gels; when it picks up moisture, ammonium sulfate-activated gel very rapidly loses its ability to resolve lecithin from phosphatidylinositol; in gel containing ammonium sulfate, small amounts of phosphatidylethanolamine are hydrolyzed to lyso-phosphatidylethanolamine.

Guilty by dissociation-development of gas chromatography-mass spectrometry (GC-MS) and other rapid screening methods for the analysis of 13 diphenidine-derived new psychoactive substances (NPSs).

PubMed

Geyer, Pierre M; Hulme, Matthew C; Irving, Joseph P B; Thompson, Paul D; Ashton, Ryan N; Lee, Robert J; Johnson, Lucy; Marron, Jack; Banks, Craig E; Sutcliffe, Oliver B

2016-11-01

The prevalence of new psychoactive substances (NPSs) in forensic casework has increased prominently in recent years. This has given rise to significant legal and analytical challenges in the identification of these substances. The requirement for validated, robust and rapid testing methodologies for these compounds is obvious. This study details the analysis of 13 synthesised diphenidine derivatives encountered in casework using presumptive testing, thin layer chromatography and gas chromatography-mass spectrometry (GC-MS). Specifically, the validated GC-MS method provides, for the first time, both a general screening method and quantification of the active components for seized solid samples, both in their pure form and in the presence of common adulterants. Graphical Abstract Chemical synthesis and forensic analysis of 13 diphenidine-derived new psychoactive substance(s).

High performance thin layer chromatography fingerprinting, phytochemical and physico-chemical studies of anti-diabetic herbal extracts

PubMed Central

Itankar, Prakash R.; Sawant, Dattatray B.; Tauqeer, Mohd.; Charde, Sonal S.

2015-01-01

Introduction: Herbal medicines have gained increasing popularity in the last few decades, and this global resurgence of herbal medicines increases their commercial value. However, this increasing demand has resulted in a decline in their quality, primarily due to a lack of adequate regulations pertaining to herbal medicines. Aim: To develop an optimized methodology for the standardization of herbal raw materials. Materials and Methods: The present study has been designed to examine each of the five herbal anti-diabetic drugs, Gymnema sylvester R. Br., Pterocarpus marsupium Roxburgh., Enicostema littorale Blume., Syzygium cumini (L.) Skeels. and Emblica officinalis Gaertn. The in-house extracts and marketed extracts were evaluated using physicochemical parameters, preliminary phytochemical screening, quantification of polyphenols (Folin–Ciocalteu colorimetric method) and high performance thin layer chromatography (HPTLC) fingerprint profiling with reference to marker compounds in plant extracts. Results: All the plants mainly contain polyphenolic compounds and are quantified in the range of 3.6–21.72% w/w. E. officinalis contain the highest and E. littorale contain the lowest content of polyphenol among plant extracts analyzed. HPTLC fingerprinting showed that the in-house extracts were of better quality than marketed extracts. Conclusion: The results obtained from the study could be utilized for setting limits for the reference phytoconstituents (biomarker) for the quality control and quality assurance of these anti-diabetic drugs. PMID:27011722

Standardisation of Gymnema sylvestre R.Br. by high-performance thin-layer chromatography: an improved method.

PubMed

Raju, Valivarthi S R; Kannababu, S; Subbaraju, Gottumukkala V

2006-01-01

An improved high-performance thin-layer chromatographic (HPTLC) method for the standardisation of Gymnema sylvestre is reported. The method involves the initial hydrolysis of gymnemic acids, the active ingredients, to a common aglycone followed by the quantitative estimation of gymnemagenin. The present method rectifies an error found in an HPTLC method reported recently.

Determination of Four Major Saponins in Skin and Endosperm of Seeds of Horse Chestnut (Aesculus Hippocastanum L.) Using High Performance Liquid Chromatography with Positive Confirmation by Thin Layer Chromatography

PubMed Central

Abudayeh, Zead Helmi Mahmoud; Al Azzam, Khaldun Mohammad; Naddaf, Ahmad; Karpiuk, Uliana Vladimirovna; Kislichenko, Viktoria Sergeevna

2015-01-01

Purpose: To separate and quantify four major saponins in the extracts of the skin and the endosperm of seeds of horse chestnut (Aesculus hippocastanum L.) using ultrasonic solvent extraction followed by a high performance liquid chromatography-diode array detector (HPLC-DAD) with positive confirmation by thin layer chromatography (TLC). Methods: The saponins: escin Ia, escin Ib, isoescin Ia and isoescin Ib were extracted using ultrasonic extraction method. The optimized extraction conditions were: 70% methanol as extraction solvent, 80 °C as extraction temperature, and the extraction time was achieved in 4 hours. The HPLC conditions used: Zorbax SB-ODS-(150 mm × 2.1 mm, 3 μm) column, acetonitrile and 0.10% phosphoric acid solution (39:61 v/v) as mobile phase, flow rate was 0.5 mL min−1 at 210 nm and 230 nm detection. The injection volume was 10 μL, and the separation was carried out isothermally at 30 °C in a heated chamber. Results: The results indicated that the developed HPLC method is simple, sensitive and reliable. Moreover, the content of escins in seeds decreased by more than 30% in endosperm and by more than 40% in skin upon storage for two years. Conclusion: This assay can be readily utilized as a quality control method for horse chestnut and other related medicinal plants. PMID:26819933

Determination of Four Major Saponins in Skin and Endosperm of Seeds of Horse Chestnut (Aesculus Hippocastanum L.) Using High Performance Liquid Chromatography with Positive Confirmation by Thin Layer Chromatography.

PubMed

Abudayeh, Zead Helmi Mahmoud; Al Azzam, Khaldun Mohammad; Naddaf, Ahmad; Karpiuk, Uliana Vladimirovna; Kislichenko, Viktoria Sergeevna

2015-11-01

To separate and quantify four major saponins in the extracts of the skin and the endosperm of seeds of horse chestnut (Aesculus hippocastanum L.) using ultrasonic solvent extraction followed by a high performance liquid chromatography-diode array detector (HPLC-DAD) with positive confirmation by thin layer chromatography (TLC). The saponins: escin Ia, escin Ib, isoescin Ia and isoescin Ib were extracted using ultrasonic extraction method. The optimized extraction conditions were: 70% methanol as extraction solvent, 80 °C as extraction temperature, and the extraction time was achieved in 4 hours. The HPLC conditions used: Zorbax SB-ODS-(150 mm × 2.1 mm, 3 μm) column, acetonitrile and 0.10% phosphoric acid solution (39:61 v/v) as mobile phase, flow rate was 0.5 mL min(-1) at 210 nm and 230 nm detection. The injection volume was 10 μL, and the separation was carried out isothermally at 30 °C in a heated chamber. The results indicated that the developed HPLC method is simple, sensitive and reliable. Moreover, the content of escins in seeds decreased by more than 30% in endosperm and by more than 40% in skin upon storage for two years. This assay can be readily utilized as a quality control method for horse chestnut and other related medicinal plants.

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

PubMed

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

Extracting elastic properties of an atomically thin interfacial layer by time-domain analysis of femtosecond acoustics

NASA Astrophysics Data System (ADS)

Chen, H.-Y.; Huang, Y.-R.; Shih, H.-Y.; Chen, M.-J.; Sheu, J.-K.; Sun, C.-K.

2017-11-01

Modern devices adopting denser designs and complex 3D structures have created much more interfaces than before, where atomically thin interfacial layers could form. However, fundamental information such as the elastic property of the interfacial layers is hard to measure. The elastic property of the interfacial layer is of great importance in both thermal management and nano-engineering of modern devices. Appropriate techniques to probe the elastic properties of interfacial layers as thin as only several atoms are thus critically needed. In this work, we demonstrated the feasibility of utilizing the time-resolved femtosecond acoustics technique to extract the elastic properties and mass density of a 1.85-nm-thick interfacial layer, with the aid of transmission electron microscopy. We believe that this femtosecond acoustics approach will provide a strategy to measure the absolute elastic properties of atomically thin interfacial layers.

Separation techniques: Chromatography

PubMed Central

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

High-performance Thin-layer Chromatography Method Development, Validation, and Simultaneous Quantification of Four Compounds Identified in Standardized Extracts of Orthosiphon stamineus.

PubMed

Hashim, Suzana; Beh, Hooi Kheng; Hamil, Mohamad Shahrul Ridzuan; Ismail, Zhari; Majid, Amin Malik Shah Abdul

2016-01-01

Orthosiphon stamineus is a medicinal herb widely grown in Southeast Asia and tropical countries. It has been used traditionally as a diuretic, abdominal pain, kidney and bladder inflammation, gout, and hypertension. This study aims to develop and validate the high-performance thin layer chromatography (HPTLC) method for quantification of rosmarinic acid (RA), 3'-hydroxy-5,6,7,4'-tetramethoxyflavone (TMF), sinensitin (SIN) and eupatorin (EUP) found in ethanol, 50% ethanol and water extract of O. stamineus leaves. HPTLC method was conducted using an HPTLC system with a developed mobile phase system of toluene: ethyl acetate: formic acid (3:7:0.1) performed on precoated silica gel 60 F254 TLC plates. The method was validated based on linearity, accuracy, precision, limit of detection, limit of quantification (LOQ), and specificity, respectively. The detection of spots was observed at ultraviolet 254 nm and 366 nm. The linearity of RA, TMF, SIN, and EUP were obtained between 10 and 100 ng/spot with high correlation coefficient value (R 2 ) of more than 0.986. The limit of detection was found to be 122.47 ± 3.95 (RA), 43.38 ± 0.79 (SIN), 17.26 ± 1.16 (TMF), and 46.80 ± 1.33 ng/spot (EUP), respectively. Whereas the LOQ was found to be 376.44 ± 6.70 (RA), 131.45 ± 2.39 (SIN), 52.30 ± 2.01 (TMF), and 141.82 ± 1.58 ng/spot (EUP), respectively. The proposed method showed good linearity, precision, accuracy, and high sensitivity. Hence, it may be applied in a routine quantification of RA, SIN, TMF, and EUP found in ethanol, 50% of ethanol and water extract of O. stamineus leaves. HPTLC method provides rapid estimation of the marker compound for routine quality control analysis.The established HPTLC method is rapid for qualitative and quantitative fingerprinting of Orthosiphon stamineus extract used for commercial product.Four identified markers (RA, SIN, EUP and TMF) found in three a different type of O. stamineus extracts specifically ethanol, 50% ethanol and water

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

PubMed

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.

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

PubMed

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/H 2 O 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 (K M ; V max ) 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.

Detection of tobacco-related biomarkers in urine samples by surface-enhanced Raman spectroscopy coupled with thin-layer chromatography.

PubMed

Huang, Rongfu; Han, Sungyub; Li, Xiao Sheryl

2013-08-01

The nicotine metabolites, cotinine and trans-3'-hydroxycotinine (3HC) are considered as superior biomarkers for identifying tobacco exposure. More importantly, the ratio of 3HC to cotinine is a good indicator to phenotype individuals for cytochrome P450 2A6 activity and to individualize pharmacotherapy for tobacco addiction. In this paper, a simple, robust and novel method based on surface-enhanced Raman spectroscopy coupled with thin-layer chromatography (TLC) was developed to directly quantify the biomarkers in human urine samples. This is the first time surface-enhanced Raman spectroscopy (SERS) was used to detect cotinine and 3HC in urine samples. The linear dynamic range for the detection of cotinine is from 40 nM to 8 μM while that of 3HC is from 1 μM to 15 μM. The detection limits are 10 nM and 0.2 μM for cotinine and 3HC, respectively. The proposed method was further validated by quantifying the concentration of both cotinine and 3HC in smokers' urine samples. This TLC-SERS method allows the direct detection of cotinine in the urine samples of both active and passive smokers and the detection of 3HC in smokers.

Super Gas Barrier Thin Films via Layer-by-Layer Assembly of Polyelectrolytes and Clay

NASA Astrophysics Data System (ADS)

Priolo, Morgan; Gamboa, Daniel; Grunlan, Jaime

2010-03-01

Thin composite films of branched polyethylenimine (PEI), polyacrylic acid (PAA) and sodium montmorillonite clay (MMT) platelets were prepared using layer-by-layer assembly. Film thickness, mass deposited per layer, and barrier were shown to increase exponentially with the number of deposition cycles. After 32 layers (i.e., eight PEI/PAA/PEI/MMT quadlayers) are deposited, the resulting transparent film exhibits an oxygen transmission rate below the detection limit of commercial instrumentation (< 0.005 cm^3/m^2 . day). This level of oxygen barrier is believed to be due to a nano-brick wall microstructure comprised of exfoliated clay bricks in polymeric mortar, where the enhanced spacing between MMT layers, provided by PEI and PAA, creates channels perpendicular concentration gradient that delay the permeating molecule. These films are good candidates for flexible electronics, food, and pharmaceutical packaging due to their transparency, super gas barrier (that rivals SiOx) and lack of metal.

Thin-layer chromatographic determination of erythromycin and other macrolide antibiotics in livestock products.

PubMed

Petz, M; Solly, R; Lymburn, M; Clear, M H

1987-01-01

A method is described for determination of 4 macrolide antibiotics in livestock products. Erythromycin, tylosin, oleandomycin, and spiramycin were extracted from animal tissues, milk, and egg with acetonitrile at pH 8.5. Cleanup was done by adding sodium chloride and dichloromethane, evaporating the organic layer, and subsequent acid/base partitioning. After the antibiotics were separated by thin-layer chromatography (TLC), they were reacted with xanthydrol and could be detected as purple spots down to 0.02 mg/kg without interference by other commonly used therapeutic drugs (23 were tested). Anisaldehyde-sulfuric acid, cerium sulfate-molybdic acid, phosphomolybdic acid, and Dragendorff's reagent proved to be less sensitive as visualizing agents. For quantitation, TLC plates were scanned at 525 nm. Recoveries were between 71 and 96% for erythromycin and tylosin in liver, muscle, and egg at the 0.1-0.5 mg/kg level and 51% for erythromycin in milk at the 0.02 mg/kg level (coefficient of variation = 10-18%). Bioautography with Bacillus subtilis was used to confirm results, in addition to TLC analysis of derivatized antibiotics and liquid chromatography with electrochemical detection. Various derivatization procedures for erythromycin were investigated for improved ultra-violet or fluorescence detection in liquid chromatography.

Oxysterols in cosmetics-Determination by planar solid phase extraction and gas chromatography-mass spectrometry.

PubMed

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.

Internal hypersonic flow. [in thin shock layer

NASA Technical Reports Server (NTRS)

Lin, T. C.; Rubin, S. G.

1974-01-01

An approach for studying hypersonic internal flow with the aid of a thin-shock-layer approximation is discussed, giving attention to a comparison of thin-shock-layer results with the data obtained on the basis of the imposition theory or a finite-difference integration of the Euler equations. Relations in the case of strong interaction are considered together with questions of pressure distribution and aspects of the boundary-layer solution.

Methods for making thin layers of crystalline materials

DOEpatents

Lagally, Max G; Paskiewicz, Deborah M; Tanto, Boy

2013-07-23

Methods for making growth templates for the epitaxial growth of compound semiconductors and other materials are provided. The growth templates are thin layers of single-crystalline materials that are themselves grown epitaxially on a substrate that includes a thin layer of sacrificial material. The thin layer of sacrificial material, which creates a coherent strain in the single-crystalline material as it is grown thereon, includes one or more suspended sections and one or more supported sections.

Structural profiling of individual glycosphingolipids in a single thin-layer chromatogram by multiple sequential immunodetection matched with Direct IR-MALDI-o-TOF mass spectrometry.

PubMed

Souady, Jamal; Soltwisch, Jens; Dreisewerd, Klaus; Haier, Jörg; Peter-Katalinić, Jasna; Müthing, Johannes

2009-11-15

The thin-layer chromatography (TLC) immunoenzyme overlay assay is a widely used tool for antibody-mediated identification of glycosphingolipids (GSLs) in mixtures. However, because the majority of GSLs is left unexamined in a chromatogram of a single assay, we developed a novel method that permits detection of various GSLs by sequential multiple immunostaining combined with individual coloring of GSLs in the same chromatogram. Specific staining was achieved by means of primary anti-GSL antibodies, directed against lactosylceramide, globotriaosylceramide, and globotetraosylceramide, in conjunction with alkaline phosphatase (AP)- or horseradish peroxidase (HRP)-conjugated secondary antibodies together with the appropriate chromogenic substrates. Triple coloring with 5-bromo-4-chloro-3-indolyl phosphate (BCIP)-AP, Fast Red-AP, and 3,3'-diaminobenzidine (DAB)-HRP resulted in blue, red, and black precipitates, respectively, following three sequential immunostaining rounds. Structures of antibody-detected GSLs were determined by direct coupling of TLC with infrared matrix-assisted laser desorption/ionization orthogonal time-of-flight mass spectrometry. This combinatorial technique was used to demonstrate structural GSL profiling of crude lipid extracts from human hepatocellular cancer. This powerful technology allows efficient structural characterization of GSLs in small tissue samples and marks a further step forward in the emerging field of glycosphingolipidomics.

Determination of Components in Beverages by Thin-Layer Chromatography.

ERIC Educational Resources Information Center

Ma, Yinfa; Yeung, Edward S.

1990-01-01

Described is a simple and interesting chromatography experiment using three different fluorescence detection principles for the determination of caffeine, saccharin and sodium benzoate in beverages. Experimental procedures and an analysis and discussion of the results are included. (CW)

Therapeutic drug monitoring of nevirapine in saliva in Uganda using high performance liquid chromatography and a low cost thin-layer chromatography technique.

PubMed

Lamorde, Mohammed; Fillekes, Quirine; Sigaloff, Kim; Kityo, Cissy; Buzibye, Allan; Kayiwa, Joshua; Merry, Concepta; Nakatudde-Katumba, Lillian; Burger, David; de Wit, Tobias F Rinke

2014-09-01

In resource limited settings access to laboratory monitoring of HIV treatment is limited and therapeutic drug monitoring is generally unavailable. This study aimed to evaluate nevirapine concentrations in saliva using low-cost thin-layer chromatography (TLC) and nevirapine concentrations in plasma and saliva using high performance liquid chromatography (HPLC) methods; and to correlate nevirapine plasma concentrations to HIV treatment outcomes in Ugandan patients. Paired plasma and stimulated saliva samples were obtained from Ugandan, HIV-infected adults on nevirapine-based ART. Nevirapine concentrations were measured using a validated HPLC method and a novel TLC method. Plasma nevirapine concentrations <3.0 mg/L using HPLC were considered subtherapeutic. Negative/positive predictive values of different thresholds for subtherapeutic nevirapine concentrations in saliva were determined. Virologic testing and, if applicable, HIV drug resistance testing was performed. Median (interquartile range, IQR) age of 297 patients was 39.1 (32.8-45.2) years. Three hundred saliva and 287 plasma samples were available for analysis. Attempts failed to determine nevirapine saliva concentrations by TLC. Using HPLC, median (IQR) nevirapine concentrations in saliva and plasma were 3.40 (2.59-4.47) mg/L and 6.17 (4.79-7.96) mg/L, respectively. The mean (coefficient of variation,%) nevirapine saliva/plasma ratio was 0.58 (62%). A cut-off value of 1.60 mg/L nevirapine in saliva was associated with a negative/positive predictive value of 0.99/0.72 and a sensitivity/specificity of 87%/98% for predicting subtherapeutic nevirapine plasma concentrations, respectively. Only 5% (15/287) of patients had subtherapeutic nevirapine plasma concentrations, of which 3 patients had viral load results > 400 copies/mL. Patients with nevirapine concentrations in plasma <3.0 mg/L had an Odds Ratio of 3.29 (95% CI: 1.00 - 10.74) for virological failure (viral load >400 copies/mL). The low-cost TLC

Evaluation of the mass transfer process on thin layer drying of papaya seeds from the perspective of diffusive models

NASA Astrophysics Data System (ADS)

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.

Recent applications of gas chromatography with high-resolution mass spectrometry.

PubMed

Špánik, Ivan; Machyňáková, Andrea

2018-01-01

Gas chromatography coupled to high-resolution mass spectrometry is a powerful analytical method that combines excellent separation power of gas chromatography with improved identification based on an accurate mass measurement. These features designate gas chromatography with high-resolution mass spectrometry as the first choice for identification and structure elucidation of unknown volatile and semi-volatile organic compounds. Gas chromatography with high-resolution mass spectrometry quantitative analyses was previously focused on the determination of dioxins and related compounds using magnetic sector type analyzers, a standing requirement of many international standards. The introduction of a quadrupole high-resolution time-of-flight mass analyzer broadened interest in this method and novel applications were developed, especially for multi-target screening purposes. This review is focused on the development and the most interesting applications of gas chromatography coupled to high-resolution mass spectrometry towards analysis of environmental matrices, biological fluids, and food safety since 2010. The main attention is paid to various approaches and applications of gas chromatography coupled to high-resolution mass spectrometry for non-target screening to identify contaminants and to characterize the chemical composition of environmental, food, and biological samples. The most interesting quantitative applications, where a significant contribution of gas chromatography with high-resolution mass spectrometry over the currently used methods is expected, will be discussed as well. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantitative determination of 3,4-methylenedioxymethamphetamine by thin-layer chromatography in ecstasy illicit pills in Tehran.

PubMed

Shetab Boushehri, Seyed Vahid; Tamimi, Maryam; Kebriaeezadeh, Abbas

2009-11-01

3,4-Methylenedioxymethamphetamine (MDMA) is the major ingredient of ecstasy illicit pills. It is a hallucinogen, central nervous system stimulant, and serotonergic neurotoxin that strongly releases serotonin from serotonergic nerves terminals. Moreover, it releases norepinephrine and dopamine from nerves terminal, but to a lesser extent than serotonin. Poisoning and even death from abusing MDMA-containing ecstasy illicit pills among abusers is usual. Thus, quantitative determination of MDMA content of ecstasy illicit pills in illicit drug bazaar must be done regularly to find the most high dose ecstasy illicit pills and removing them from illicit drug bazaar. In the present study, MDMA contents of 13 most abundant ecstasy illicit pills were determined by quantitative thin-layer chromatography (TLC). Two procedures for quantitative determination of MDMA contents of ecstasy illicit pills by TLC were used: densitometric and so-called 'scraping off' methods. The former was done in a reflection mode at 285 nm and the latter was done by absorbance measurement of eluted scraped off spots. Limit of detection (LOD), considering signal-to-noise ratio (S/N) of 2, and limit of quantification (LOQ), regarding S/N of 10, of densitometric and scraping off methods were 0.40 microg, 1.20 microg, and 6.87 mug, 20.63 microg, respectively. Repeatabilities (within-laboratory error) of densitometric and scraping off methods were 0.5% and 3.6%, respectively. The results showed that the ecstasy illicit pills contained 24-124.5 mg and 23.9-122.2 mg MDMA by densitometric and scraping off methods, respectively.

Positional isomerization of trans-3-hexadecenoic acid employing 2-amino-2-methyl-propanol as a derivatizing agent for ethylenic bond location by gas chromatography/mass spectrometry.

PubMed

Lamberto, M; Ackman, R G

1995-09-20

The effect of derivatization with 2-amino-2-methyl-propanol on trans-3-hexadecenoic acid was investigated as part of the identification of the trans-3-hexadecenoic acid in two Nova Scotian seaweeds. After the extraction of the total fatty acids and their methylation, the monoenoic trans fraction was isolated by thin-layer chromatography on silica gels impregnated with silver nitrate. This fraction was first analyzed by gas chromatography and showed the presence of the trans-3-hexadecenoic acid; other fatty acids were not present. The isolated fraction was derivatized with 2-amino-2-methyl-propanol prior to analysis by gas chromatography/mass spectrometry. The chromatogram obtained showed the presence of a positional isomer formed during the derivatization of the trans-3-hexadecenoic acid. The mass spectrum showed a prominent [M+H] and diagnostic ions for the identification of the unknown isomer, corresponding to the 4,4-dimethyloxazoline (DMOX) derivative of a presumed 2-hexadecenoic acid. Definitive confirmation of the ethylenic bond position was obtained by oxidative ozonolysis of the DMOX derivatives of the fatty acids under investigation. Infrared spectroscopy showed that the artifact formed during the DMOX derivatization of trans-3-hexadecenoic acid was the DMOX derivative of cis-2-hexadecenoic acid.

Role of thin-layer chromatography in ascertaining Kashaya Rasa (astringent taste) in medicinal plants on the concept of Samana and Vichitra Pratyayarabdha principles of Ayurveda

PubMed Central

Kolhe, Rasika H.; Acharya, Rabinarayan; Shukla, Vinay J.

2014-01-01

Background: Pharmacodynamics, in Ayurveda has been described in terms of Rasadipanchaka. Rasa, on one side indicates the Bhautika composition of the drug and on the other side predicts the action. Different analytical techniques, pharmaceutical processes are being used in Ayurveda for the purpose of standardization of raw drugs. Aim: In this study an attempt has been made to apply chromatographic technique in determination of Kashaya (astringent) Rasa (taste). Materials and Methods: Two important Kashaya dominant drugs Kulattha (Dolichos biflorus Linn.) and Kanchanara (Bauhinia variegata Linn.), falling under Vichitra and Samana Pratyayarabdha category respectively, were subjected to physicochemical parameters and qualitative tests followed by High-Performance Thin-Layer Chromatography (HPTLC). In light of chromatographic fingerprinting; sample preparation protocol is modified to incorporate taste threshold in correlation. Column chromatography is used for first-level discrimination technique followed by HPTLC. Kashaya Rasa Dominant Zone (KsRDZ) was separated and subjected to TLC fingerprinting. The KsRDZ fraction was designated as Botanical Reference Material (BRM) in further analysis. Results: Ash value, Alcohol and water soluble extract value were more in B variegata as compared to D biflorus. Presence of tannin in both the samples was confirmed through qualitative test. The KsRDZ fraction separated at Rf 0.46 and 0.48 for Kulattha and Kanchanara respectively. Conclusion: The results showed that the planner chromatography technique seems very useful when BRM hypothesis was adjunct to method that explains the categorization according to traditional Rasa domain classification method. PMID:25558164

Modeling of Multiphase Flow through Thin Porous Layers: Application to a Polymer Electrolyte Fuel Cell (PEFC)

NASA Astrophysics Data System (ADS)

Qin, C.; Hassanizadeh, S.

2013-12-01

number of material properties in the model need to be determined experimentally, such as mass and heat exchange coefficients between neighboring layers. Fig. 1: Schematic representation of three thin porous layers, which may exchange mass, momentum, and energy. Also, a typical averaging domain (REV) is shown. Note that the layer thickness and thus the REV height can be spatially variable. Also, in reality, the layers are tightly stacked and there is no gap between them.

Fast liquid chromatography combined with mass spectrometry for the analysis of metabolites and proteins in human body fluids.

PubMed

Kortz, Linda; Helmschrodt, Christin; Ceglarek, Uta

2011-03-01

In the last decade various analytical strategies have been established to enhance separation speed and efficiency in high performance liquid chromatography applications. Chromatographic supports based on monolithic material, small porous particles, and porous layer beads have been developed and commercialized to improve throughput and separation efficiency. This paper provides an overview of current developments in fast chromatography combined with mass spectrometry for the analysis of metabolites and proteins in clinical applications. Advances and limitations of fast chromatography for the combination with mass spectrometry are discussed. Practical aspects of, recent developments in, and the present status of high-throughput analysis of human body fluids for therapeutic drug monitoring, toxicology, clinical metabolomics, and proteomics are presented.

Free and bound excitons in thin wurtzite GaN layers on sapphire

NASA Astrophysics Data System (ADS)

Merz, C.; Kunzer, M.; Kaufmann, U.; Akasaki, I.; Amano, H.

1996-05-01

Free and bound excitons have been studied by photoluminescence in thin (0268-1242/11/5/010/img8) wurtzite-undoped GaN, n-type GaN:Si as well as p-type GaN:Mg and GaN:Zn layers grown by metal-organic chemical vapour phase deposition (MOCVD). An accurate value for the free A exciton binding energy and an estimate for the isotropically averaged hole mass of the uppermost 0268-1242/11/5/010/img9 valence band are deduced from the data on undoped samples. The acceptor-doped samples reveal recombination lines which are attributed to excitons bound to 0268-1242/11/5/010/img10 and 0268-1242/11/5/010/img11 respectively. These lines are spectrally clearly separated and the exciton localization energies are in line with Haynes' rule. Whenever a comparison is possible, it is found that the exciton lines in these thin MOCVD layers are ultraviolet-shifted by 20 to 25 meV as compared to quasi-bulk (0268-1242/11/5/010/img12) samples. This effect is interpreted in terms of the compressive hydrostatic stress component which thin GaN layers experience when grown on sapphire with an AlN buffer layer.

Slantingly cross loading sample system enables simultaneous performance of separation and mixture to detect molecular interactions on thin-layer chromatography.

PubMed

Shimizu-Yumoto, Hiroko; Hayashi, Nobuyuki; Ichimura, Kazuo; Nakayama, Masayoshi

2012-07-06

Anthocyanins are major flower pigments that can be affected by copigments, colorless compounds that can modify anthocyanin coloration to more intense and bluer. Thin-layer chromatography (TLC) is an available technique to separate and analyze anthocyanins and copigments. To easily and comprehensively detect copigments, we added function of mixture of compounds to TLC; by slantingly cross loading samples on TLC, compounds are symmetrically developed at various angle lines from the upper origin to individual R(f) values and cross each other in an orderly fashion, where mixture is simultaneously performed with separation. Occurrence of copigments can be detected as a coloration change on the developed line of anthocyanin. Pink sweet pea (Lathyrus odoratus L.) petals were analyzed by the cross-TLC and a more intense spot and a paler spot on the anthocyanin line were detected. As each spot overlapped with an ultraviolet absorbance line, each of these ultraviolet absorption compounds was purified and identified as kaempferol 3-rhamnoside and 2-cyanoethyl-isoxazolin-5-one, respectively. Whereas kaempferol 3-rhamnoside is a flavonoid and had a general copigment effect of more intense and bluer coloration change, 2-cyanoethyl-isoxazolin-5-one is a compound whose structure is outside of conventional categories of copigments and had a novel effect to change anthocyanin coloration paler while maintaining color tone. We determined that the search for copigments should be carried out without pre-existing prediction of structures and effects. We have shown that slantingly cross loading samples system on plate-type chromatography is an effective technique for such comprehensive analysis of molecular interaction. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

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

USDA-ARS?s Scientific Manuscript database

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...

Voltammetric Thin-Layer Ionophore-Based Films: Part 2. Semi-Empirical Treatment.

PubMed

Yuan, Dajing; Cuartero, Maria; Crespo, Gaston A; Bakker, Eric

2017-01-03

This work reports on a semiempirical treatment that allows one to rationalize and predict experimental conditions for thin-layer ionophore-based films with cation-exchange capacity read out with cyclic voltammetry. The transition between diffusional mass transport and thin-layer regime is described with a parameter (α), which depends on membrane composition, diffusion coefficient, scan rate, and electrode rotating speed. Once the thin-layer regime is fulfilled (α = 1), the membrane behaves in some analogy to a potentiometric sensor with a second discrimination variable (the applied potential) that allows one to operate such electrodes in a multianalyte detection mode owing to the variable applied ion-transfer potentials. The limit of detection of this regime is defined with a second parameter (β = 2) and is chosen in analogy to the definition of the detection limit for potentiometric sensors provided by the IUPAC. The analytical equations were validated through the simulation of the respective cyclic voltammograms under the same experimental conditions. While simulations of high complexity and better accuracy satisfactorily reproduced the experimental voltammograms during the forward and backward potential sweeps (companion paper 1), the semiempirical treatment here, while less accurate, is of low complexity and allows one to quite easily predict relevant experimental conditions for this emergent methodology.

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

ERIC Educational Resources Information Center

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…

Chemometrics comparison of gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry Daphnia magna metabolic profiles exposed to salinity.

PubMed

Parastar, Hadi; Garreta-Lara, Elba; Campos, Bruno; Barata, Carlos; Lacorte, Silvia; Tauler, Roma

2018-06-01

The performances of gas chromatography with mass spectrometry and of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry are examined through the comparison of Daphnia magna metabolic profiles. Gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with mass spectrometry were used to compare the concentration changes of metabolites under saline conditions. In this regard, a chemometric strategy based on wavelet compression and multivariate curve resolution-alternating least squares is used to compare the performances of gas chromatography with mass spectrometry and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry for the untargeted metabolic profiling of Daphnia magna in control and salinity-exposed samples. Examination of the results confirmed the outperformance of comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry over gas chromatography with mass spectrometry for the detection of metabolites in D. magna samples. The peak areas of multivariate curve resolution-alternating least squares resolved elution profiles in every sample analyzed by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry were arranged in a new data matrix that was then modeled by partial least squares discriminant analysis. The control and salt-exposed daphnids samples were discriminated and the most relevant metabolites were estimated using variable importance in projection and selectivity ratio values. Salinity de-regulated 18 metabolites from metabolic pathways involved in protein translation, transmembrane cell transport, carbon metabolism, secondary metabolism, glycolysis, and osmoregulation. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

ERIC Educational Resources Information Center

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…

Sound transmission through finite lightweight multilayered structures with thin air layers.

PubMed

Dijckmans, A; Vermeir, G; Lauriks, W

2010-12-01

The sound transmission loss (STL) of finite lightweight multilayered structures with thin air layers is studied in this paper. Two types of models are used to describe the vibro-acoustic behavior of these structures. Standard transfer matrix method assumes infinite layers and represents the plane wave propagation in the layers. A wave based model describes the direct sound transmission through a rectangular structure placed between two reverberant rooms. Full vibro-acoustic coupling between rooms, plates, and air cavities is taken into account. Comparison with double glazing measurements shows that this effect of vibro-acoustic coupling is important in lightweight double walls. For infinite structures, structural damping has no significant influence on STL below the coincidence frequency. In this frequency region, the non-resonant transmission or so-called mass-law behavior dominates sound transmission. Modal simulations suggest a large influence of structural damping on STL. This is confirmed by experiments with double fiberboard partitions and sandwich structures. The results show that for thin air layers, the damping induced by friction and viscous effects at the air gap surfaces can largely influence and improve the sound transmission characteristics.

Layer-by-Layer Assembly of a pH-Responsive and Electrochromic Thin Film

ERIC Educational Resources Information Center

Schmidt, Daniel J.; Pridgen, Eric M.; Hammond, Paula T.; Love, J. Christopher

2010-01-01

This article summarizes an experiment on thin-film fabrication with layer-by-layer assembly that is appropriate for undergraduate laboratory courses. The purpose of this experiment is to teach students about self-assembly in the context of thin films and to expose students to the concepts of functional polymeric coatings. Students dip coat…

MultiLayer solid electrolyte for lithium thin film batteries

DOEpatents

Lee, Se -Hee; Tracy, C. Edwin; Pitts, John Roland; Liu, Ping

2015-07-28

A lithium metal thin-film battery composite structure is provided that includes a combination of a thin, stable, solid electrolyte layer [18] such as Lipon, designed in use to be in contact with a lithium metal anode layer; and a rapid-deposit solid electrolyte layer [16] such as LiAlF.sub.4 in contact with the thin, stable, solid electrolyte layer [18]. Batteries made up of or containing these structures are more efficient to produce than other lithium metal batteries that use only a single solid electrolyte. They are also more resistant to stress and strain than batteries made using layers of only the stable, solid electrolyte materials. Furthermore, lithium anode batteries as disclosed herein are useful as rechargeable batteries.

Buffer layers for high-Tc thin films on sapphire

NASA Technical Reports Server (NTRS)

Wu, X. D.; Foltyn, S. R.; Muenchausen, R. E.; Cooke, D. W.; Pique, A.; Kalokitis, D.; Pendrick, V.; Belohoubek, E.

1992-01-01

Buffer layers of various oxides including CeO2 and yttrium-stabilized zirconia (YSZ) have been deposited on R-plane sapphire. The orientation and crystallinity of the layers were optimized to promote epitaxial growth of YBa2Cu3O(7-delta) (YBCO) thin films. An ion beam channeling minimum yield of about 3 percent was obtained in the CeO2 layer on sapphire, indicating excellent crystallinity of the buffer layer. Among the buffer materials used, CeO2 was found to be the best one for YBCO thin films on R-plane sapphire. High Tc and Jc were obtained in YBCO thin films on sapphire with buffer layers. Surface resistances of the YBCO films were about 4 mOmega at 77 K and 25 GHz.

Factitious diarrhea induced by stimulant laxatives: accuracy of diagnosis by a clinical reference laboratory using thin layer chromatography.

PubMed

Shelton, Joseph H; Santa Ana, Carol A; Thompson, Donald R; Emmett, Michael; Fordtran, John S

2007-01-01

Surreptitious ingestion of laxatives can lead to serious factitious diseases that are difficult to diagnose. Most cases involve ingestion of bisacodyl or senna. Thin layer chromatography (TLC) of urine or stool is the only commercially available test for these laxatives. Such testing is considered highly reliable, but its accuracy in clinical practice is unknown. Our aim was to evaluate the reliability of TLC laxative testing by a clinical reference laboratory in the United States. Diarrhea was induced in healthy volunteers by ingestion of bisacodyl, senna, or a control laxative (n = 11 for each laxative group). Samples of urine and diarrheal stool were sent in blinded fashion to the clinical reference laboratory for bisacodyl and senna analysis. TLC testing for bisacodyl-induced diarrhea revealed a sensitivity of 73% and specificity of 91% when urine was tested and sensitivity and specificity of 91% and 96%, respectively, when stool was analyzed. When diarrhea was induced by senna, the TLC assay for senna failed to identify even a single urine or stool specimen as positive (zero% sensitivity). Considering the expected prevalence of surreptitious laxative abuse in patients with chronic idiopathic diarrhea (2.4%-25%, depending on the clinical setting), TLC of urine or stool for bisacodyl by this reference laboratory would often produce misleading results, and testing for senna would have no clinical value. The major problems are false-positive tests for bisacodyl and false-negative tests for senna.

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

PubMed

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.

Determination of exogenous epigallocatechin gallate peracetate in mouse plasma using liquid chromatography with quadrupole time-of-flight mass spectrometry.

PubMed

Chu, Kai On; Man, Gene Chi Wai; Chan, Kwok Ping; Chu, Ching Yan; Chan, Tak Hang; Pang, Chi Pui; Wang, Chi Chiu

2014-12-01

A robust method for the quantitation of epigallocatechin gallate peracetate in plasma for pharmacokinetic studies is lacking. We have developed a validated method to quantify this compound using liquid chromatography with quadrupole time-of-flight mass spectrometry with isopropanol and tert-butyl methyl ether (3:10) extraction and thin-layer chromatography purification. The epigallocatechin gallate peracetate-1-(13) C8 isotope was used as an internal standard. The linear range (r(2) > 0.9950) was from 0.05 to 100.00 μg/mL. The lower limit of quantification of the method was 0.05 μg/mL. Reproducibility, coefficient of variation, was between 0.7 and 12.6% (n = 6), accuracy between 83.7 and 104.6% (n = 5), and recovery ranged from 82.4 to 109.0% (n = 4). Ion suppression was approximately 40%. No mass spectral peaks were found to interfere between the standard and internal standard or the blank plasma extracts. Epigallocatechin gallate peracetate in plasma was stably stored at -80°C over three months even after three freeze-thaw cycles. Extracts were stable in the sampler at 4°C for over 48 h. Plasma levels were maintained at 1.36 μg/mL for 360 min after intraorbital intravenous injection at 50 mg/kg in mice. This method can be used to reliably measure epigallocatechin gallate peracetate in plasma for pharmacokinetic studies. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid Crystals in Chromatography

NASA Astrophysics Data System (ADS)

Witkiewicz, Zygfryd

The following sections are included: * INTRODUCTION * LIQUID CRYSTALS SUITABLE FOR GAS CHROMATOGRAPHY * Monomeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Polymeric Liquid Crystal Stationary Phases * Conventional Analytical Columns * Capillary Columns * FACTORS AFFECTING THE CHROMATOGRAPHIC SEPARATIONS ON LIQUID CRYSTAL STATIONARY PHASES * Kind of Mesophase of the Liquid Crystal * Molecular Structure of the Liquid Crystals and of the Chromatographed Substances * Substrate on which the Liquid Crystal is Deposited * ANALYTICAL APPLICATIONS OF LIQUID CRYSTAL STATIONARY PHASES IN GAS CHROMATOGRAPHY * Separation of Isomers of Benzene and Naphthalene Derivatives * Separation of Alkane and Alkene Isomers * Separation of Mixtures of Benzene and Aliphatic Hydrocarbon Derivatives Containing Heteroatoms * Separation of Polynuclear Hydrocarbons * INVESTIGATION OF THE PROPERTIES OF LIQUID CRYSTALS BY GAS CHROMATOGRAPHY * APPLICATION OF LIQUID CRYSTALS IN LIQUID CHROMATOGRAPHY * Column Chromatography * Thin-Layer Chromatography * APPLICATION OF LIQUID CRYSTAL STATIONARY PHASES IN SUPERCRITICAL FLUID CHROMATOGRAPHY * FINAL REMARKS * References

Determination of stoichiometry and concentration of trace elements in thin BaxSr1-xTiO3 perovskite layers.

PubMed

Becker, J S; Boulyga, S F

2001-07-01

This paper describes an analytical procedure for determining the stoichiometry of BaxSr1-xTiO3 perovskite layers using inductively coupled plasma mass spectrometry (ICP-MS). The analytical results of mass spectrometry measurements are compared to those of X-ray fluorescence analysis (XRF). The performance and the limits of solid-state mass spectrometry analytical methods for the surface analysis of thin BaxSr1-xTiO3 perovskite layers sputtered neutral mass spectrometry (SNMS)--are investigated and discussed.

delta 13C analyses of vegetable oil fatty acid components, determined by gas chromatography--combustion--isotope ratio mass spectrometry, after saponification or regiospecific hydrolysis.

PubMed

Woodbury, S E; Evershed, R P; Rossell, J B

1998-05-01

The delta 13C values of the major fatty acids of several different commercially important vegetable oils were measured by gas chromatography--combustion--isotope ratio mass spectrometry. The delta 13C values obtained were found to fall into two distinct groups, representing the C3 and C4 plants classes from which the oils were derived. The delta 13C values of the oils were measured by continuous flow elemental isotope ratio mass spectrometry and were found to be similar to their fatty acids, with slight differences between individual fatty acids. Investigations were then made into the influence on the delta 13C values of fatty acids of the position occupied on the glycerol backbone. Pancreatic lipase was employed to selectively hydrolyse fatty acids from the 1- and 3-positions with the progress of the reaction being followed by high-temperature gas chromatography in order to determine the optimum incubation time. The 2-monoacylglycerols were then isolated by thin-layer chromatography and fatty acid methyl esters prepared. The delta 13C values obtained indicate that fatty acids from any position on the glycerol backbone are isotopically identical. Thus, whilst quantification of fatty acid composition at the 2-position and measurement of delta 13C values of oils and their major fatty acids are useful criteria in edible oil purity assessment, measurement of delta 13C values of fatty acids from the 2-position does not assist with oil purity assignments.

Thin layer chromatographic method for the detection of uric acid: collaborative study.

PubMed

Thrasher, J J; Abadie, A

1978-07-01

A collaborative study has been completed on an improved method for the detection and confirmation of uric acid from bird and insect excreta. The proposed method involves the lithium carbonate solubilization of the suspect excreta material, followed by butanol-methanol-water-acetic acid thin layer chromatography, and trisodium phosphate-phosphotungstic acid color development. The collaborative tests resulted in 100% detection of uric acid standard at the 50 ng level and 75% detection at the 20-25 ng level. No false positives were reported during tests of compounds similar to uric acid. The proposed method has been adopted official first action; the present official final action method, 44.161, will be retained for screening purposes.

Combined liquid chromatography-mass spectrometry for trace analysis of pharmaceuticals

NASA Astrophysics Data System (ADS)

Schmidt, Lothar; Danigel, Harald; Jungclas, Hartmut

1982-07-01

A 252Cf-plasma desorption mass spectrometer (PDMS) for the analysis of thin layers from nonvolatile organic samples has been set up to be combined with a liquid chromatograph. A novel interface performs the direct inlet of the liquid sample through a capillary into the vacuum system of the spectrometer. Samples of drugs are periodically collected, transferred to the ion source and analysed using a rotating disk. This on-line sample preparation has been tested for three antiarrhythmic drugs using various solvents and mixtures.

QUALITY ASSURANCE STUDY OF MARINE LIPID CLASS DETERMINATION USING CHROMAROD/IATROSCAN( REG. TRADEMARK) THIN-LAYER CHROMATOGRAPHY-FLAME IONIZATION DETECTOR

EPA Science Inventory

An Iatroscan thin-layer chromatorgraphy-flame ionization detector has been utilized to quantify lipid classes in marine samples. This method was evaluated relative to established quality assurance (QA) procedures used for the gas chromatographic analysis of PCBs. A method for ext...

NMR of thin layers using a meanderline surface coil

DOEpatents

Cowgill, Donald F.

2001-01-01

A miniature meanderline sensor coil which extends the capabilities of nuclear magnetic resonance (NMR) to provide analysis of thin planar samples and surface layer geometries. The sensor coil allows standard NMR techniques to be used to examine thin planar (or curved) layers, extending NMRs utility to many problems of modern interest. This technique can be used to examine contact layers, non-destructively depth profile into films, or image multiple layers in a 3-dimensional sense. It lends itself to high resolution NMR techniques of magic angle spinning and thus can be used to examine the bonding and electronic structure in layered materials or to observe the chemistry associated with aging coatings. Coupling this sensor coil technology with an arrangement of small magnets will produce a penetrator probe for remote in-situ chemical analysis of groundwater or contaminant sediments. Alternatively, the sensor coil can be further miniaturized to provide sub-micron depth resolution within thin films or to orthoscopically examine living tissue. This thin-layer NMR technique using a stationary meanderline coil in a series-resonant circuit has been demonstrated and it has been determined that the flat meanderline geometry has about he same detection sensitivity as a solenoidal coil, but is specifically tailored to examine planar material layers, while avoiding signals from the bulk.

An Electrochemical Experiment Using an Optically Transparent Thin Layer Electrode

ERIC Educational Resources Information Center

DeAngelis, Thomas P.; Heineman, William R.

1976-01-01

Describes a unified experiment in which an optically transparent thin layer electrode is used to illustrate the techniques of thin layer electrochemistry, cyclic voltammetry, controlled potential coulometry, and spectroelectrochemistry. (MLH)

Methods for producing thin film charge selective transport layers

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

Hammond, Scott Ryan; Olson, Dana C.; van Hest, Marinus Franciscus Antonius Maria

Methods for producing thin film charge selective transport layers are provided. In one embodiment, a method for forming a thin film charge selective transport layer comprises: providing a precursor solution comprising a metal containing reactive precursor material dissolved into a complexing solvent; depositing the precursor solution onto a surface of a substrate to form a film; and forming a charge selective transport layer on the substrate by annealing the film.

[A thin-layer chromatography method for determining the styrene metabolites mandelic and phenylglyoxylic acid in urine].

PubMed

Gartzke, J; Burck, D

1989-06-01

A thin-layer chromatographic method is described for the determination of mandelic and phenyglyoxillic acid on silicagel (Silufol UV 254) after extraction from urine of styrene exposed workers. The quantitative determination was performed after eluting the spots. Phenylglyoxilic acid was measured at 255 nm and mandelic acid by derivative spectroscopically estimation of the .CH(OH).COOH -chromophore at 217 nm or by a three-wavelength mode, respectively. The recovery in urine was 80-104% for phenylglyoxilic acid and 99-105% for mandelic acid.

Electrochemical oxidation and protein adduct formation of aniline: a liquid chromatography/mass spectrometry study.

PubMed

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

Combined computational-experimental approach to predict blood-brain barrier (BBB) permeation based on "green" salting-out thin layer chromatography supported by simple molecular descriptors.

PubMed

Ciura, Krzesimir; Belka, Mariusz; Kawczak, Piotr; Bączek, Tomasz; Markuszewski, Michał J; Nowakowska, Joanna

2017-09-05

The objective of this paper is to build QSRR/QSAR model for predicting the blood-brain barrier (BBB) permeability. The obtained models are based on salting-out thin layer chromatography (SOTLC) constants and calculated molecular descriptors. Among chromatographic methods SOTLC was chosen, since the mobile phases are free of organic solvent. As consequences, there are less toxic, and have lower environmental impact compared to classical reserved phases liquid chromatography (RPLC). During the study three stationary phase silica gel, cellulose plates and neutral aluminum oxide were examined. The model set of solutes presents a wide range of log BB values, containing compounds which cross the BBB readily and molecules poorly distributed to the brain including drugs acting on the nervous system as well as peripheral acting drugs. Additionally, the comparison of three regression models: multiple linear regression (MLR), partial least-squares (PLS) and orthogonal partial least squares (OPLS) were performed. The designed QSRR/QSAR models could be useful to predict BBB of systematically synthesized newly compounds in the drug development pipeline and are attractive alternatives of time-consuming and demanding directed methods for log BB measurement. The study also shown that among several regression techniques, significant differences can be obtained in models performance, measured by R 2 and Q 2 , hence it is strongly suggested to evaluate all available options as MLR, PLS and OPLS. Copyright © 2017 Elsevier B.V. All rights reserved.

Application of 2-Trichloromethylbenzimidazole in Analytical Chemistry: A Highly Selective Chromogenic Reagent for Thin-Layer Chromatography and Some Other Analytical Uses

PubMed Central

Konopski, Leszek; Kiełczewska, Anna

2012-01-01

2-Trichloromethylbenzimidazole (TCMB) was used as a chromogenic reagent in organic or inorganic analysis, mainly in thin-layer chromatography (TLC). In reactions of TCMB with some heteroaromatic nitrogen containing compounds, such as azines, azoles and benzazoles, a formation of high colored products occurred. For azines, the chromogenic reaction was highly regioselective, since the both adjacent α-positions versus the nitrogen atom(s) must not be substituted. A TLC method of detection was developed. Thirty azines, azoles, and benzazoles were detected at the detection limit 10 ng to 1 μg. This method was also applied for detection of heteroaromatic pesticides, and the attempts to construct active and passive dosimeters for nicotine were made. In a prechromatographic reaction of aromatic o-diamines with methyl trichloroacetimidate, TCMB or its derivatives were formed in situ. Followed by TLC and visualization in pyridine vapors, this procedure was applied for detection of o-phenylenediamine derivatives. The reaction product of TCMB and pyridine (LI Complex) was identified and fully characterized. Two different reaction mechanisms: with electron deficient basic heteroaromatic compounds, like pyridine, and with more acidic compounds, for example, pyrrole, were discussed. In aqueous solutions, the LI Complex may be also used as a new indicator for complexometric, adsorption and acid-base titration of inorganic compounds. PMID:22567563

Comparison Between Navier-Stokes and Thin-Layer Computations for Separated Supersonic Flow

NASA Technical Reports Server (NTRS)

Degani, David; Steger, Joseph L.

1983-01-01

In the numerical simulation of high Reynolds-number flow, one can frequently supply only enough grid points to resolve the viscous terms in a thin layer. As a consequence, a body-or stream-aligned coordinate system is frequently used and viscous terms in this direction are discarded. It is argued that these terms cannot be resolved and computational efficiency is gained by their neglect. Dropping the streamwise viscous terms in this manner has been termed the thin-layer approximation. The thin-layer concept is an old one, and similar viscous terms are dropped, for example, in parabolized Navier-Stokes schemes. However, such schemes also make additional assumptions so that the equations can be marched in space, and such a restriction is not usually imposed on a thin-layer model. The thin-layer approximation can be justified in much the same way as the boundary-layer approximation; it requires, therefore, a body-or stream-aligned coordinate and a high Reynolds number. Unlike the boundary-layer approximation, the same equations are used throughout, so there is no matching problem. Furthermore, the normal momentum equation is not simplified and the convection terms are not one-sided differenced for marching. Consequently, the thin-layer equations are numerically well behaved at separation and require no special treatment there. Nevertheless, the thin-layer approximation receives criticism. It has been suggested that the approximation is invalid at separation and, more recently, that it is inadequate for unsteady transonic flow. Although previous comparisons between the thin-layer and Navier-Stokes equations have been made, these comparisons have not been adequately documented.

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

PubMed

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.

Comparative chromatography of chloroplast pigment

NASA Technical Reports Server (NTRS)

Grandolfo, M.; Sherma, J.; Strain, H. H.

1969-01-01

Methods for isolation of low concentration pigments of the cocklebur species are described. The methods entail two step chromatography so that the different sorption properties of the various pigments in varying column parameters can be utilized. Columnar and thin layer methods are compared. Many conditions influence separability of the chloroplasts.

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

PubMed Central

Santhana Lakshmi, Karunanidhi; Lakshmi, Sivasubramanian

2012-01-01

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 (v/v/v/v) as mobile phase. Zones were scanned densitometrically at 254 nm. The R f 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. PMID:22567550

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

PubMed

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.

Productivity correlated to photobiochemical performance of Chlorella mass cultures grown outdoors in thin-layer cascades.

PubMed

Masojídek, Jiří; Kopecký, Jiří; Giannelli, Luca; Torzillo, Giuseppe

2011-02-01

This work aims to: (1) correlate photochemical activity and productivity, (2) characterize the flow pattern of culture layers and (3) determine a range of biomass densities for high productivity of the freshwater microalga Chlorella spp., grown outdoors in thin-layer cascade units. Biomass density, irradiance inside culture, pigment content and productivity were measured in the microalgae cultures. Chlorophyll-fluorescence quenching was monitored in situ (using saturation-pulse method) to estimate photochemical activities. Photobiochemical activities and growth parameters were studied in cultures of biomass density between 1 and 47 g L(-1). Fluorescence measurements showed that diluted cultures (1-2 g DW L(-1)) experienced significant photostress due to inhibition of electron transport in the PSII complex. The highest photochemical activities were achieved in cultures of 6.5-12.5 g DW L(-1), which gave a maximum daylight productivity of up to 55 g dry biomass m(-2) day(-1). A midday depression of maximum PSII photochemical yield (F (v)/F (m)) of 20-30% compared with morning values in these cultures proved to be compatible with well-performing cultures. Lower or higher depression of F (v)/F (m) indicated low-light acclimated or photo-inhibited cultures, respectively. A hydrodynamic model of the culture demonstrated highly turbulent flow allowing rapid light/dark cycles (with frequency of 0.5 s(-1)) which possibly match the turnover of the photosynthetic apparatus. These results are important from a biotechnological point of view for optimisation of growth of outdoor microalgae mass cultures under various climatic conditions.

Nonenzymatic detection of glucose using BaCuO2 thin layer

NASA Astrophysics Data System (ADS)

Ito, Takeshi; Asada, Tsuyoshi; Asai, Naoto; Shimizu, Tomohiro; Shingubara, Shoso

2017-01-01

A BaCuO2 thin layer was deposited on a glassy carbon electrode and used for the direct oxidation of glucose. The crystalline, electrochemical, and physicochemical properties that depend on the deposition temperature and deposition time were studied. X-ray diffraction (XRD) analysis showed that the thin layer was amorphous even at 400 °C. The current density of the glucose oxidation using the thin layer deposited at 200 °C was higher than those at other deposition temperatures. Under this condition, the current density increased with the glucose concentration and deposition time. These results indicate that a BaCuO2 thin layer has potential for measuring the blood glucose level without enzymes.

Thin-Layer Fuel Cell for Teaching and Classroom Demonstrations

ERIC Educational Resources Information Center

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…

Carbon-Nanotube Conductive Layers for Thin-Film Solar Cells

NASA Technical Reports Server (NTRS)

Landis, Geoffrey A.

2005-01-01

Thin, transparent layers comprising mats of carbon nanotubes have been proposed for providing lateral (that is, inplane) electrical conductivities for collecting electric currents from the front surfaces of the emitter layers of thin-film solar photovoltaic cells. Traditionally, thin, semitransparent films of other electrically conductive materials (usually, indium tin oxide, zinc oxide, or cadmium sulfide) have been used for this purpose. As in the cases of the traditional semitransparent conductive films, the currents collected by the nanotube layers would, in turn, be further collected by front metal contact stripes. Depending on details of a specific solar-cell design, the layer of carbon nanotubes would be deposited in addition to, or instead of, a semitransparent layer of one of these traditional conductive materials (see figure). The proposal is expected to afford the following advantages: The electrical conductivity of the carbon- nanotube layer would exceed that of the corresponding semitransparent layer of traditional electrically conductive material. The greater electrical conductivity of the carbon-nanotube layer would make it possible to retain adequate lateral electrical conductivity while reducing the thickness of, or eliminating entirely, the traditional semitransparent conductive layer. As a consequence of thinning or elimination of the traditional semitransparent conductive layer, less light would be absorbed, so that more of the incident light would be available for photovoltaic conversion. The greater electrical conductivity of the carbon-nanotube layer would make it possible to increase the distance between front metal contact stripes, in addition to (or instead of) thinning or eliminating the layer of traditional semitransparent conductive material. Consequently, the fraction of solar-cell area shadowed by front metal contact stripes would be reduced again, making more of the incident light available for photovoltaic conversion. The electrical

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

NASA Astrophysics Data System (ADS)

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).

Thin layer model for nonlinear evolution of the Rayleigh-Taylor instability

NASA Astrophysics Data System (ADS)

Zhao, K. G.; Wang, L. F.; Xue, C.; Ye, W. H.; Wu, J. F.; Ding, Y. K.; Zhang, W. Y.

2018-03-01

On the basis of the thin layer approximation [Ott, Phys. Rev. Lett. 29, 1429 (1972)], a revised thin layer model for incompressible Rayleigh-Taylor instability has been developed to describe the deformation and nonlinear evolution of the perturbed interface. The differential equations for motion are obtained by analyzing the forces (the gravity and pressure difference) of fluid elements (i.e., Newton's second law). The positions of the perturbed interface are obtained from the numerical solution of the motion equations. For the case of vacuum on both sides of the layer, the positions of the upper and lower interfaces obtained from the revised thin layer approximation agree with that from the weakly nonlinear (WN) model of a finite-thickness fluid layer [Wang et al., Phys. Plasmas 21, 122710 (2014)]. For the case considering the fluids on both sides of the layer, the bubble-spike amplitude from the revised thin layer model agrees with that from the WN model [Wang et al., Phys. Plasmas 17, 052305 (2010)] and the expanded Layzer's theory [Goncharov, Phys. Rev. Lett. 88, 134502 (2002)] in the early nonlinear growth regime. Note that the revised thin layer model can be applied to investigate the perturbation growth at arbitrary Atwood numbers. In addition, the large deformation (the large perturbed amplitude and the arbitrary perturbed distributions) in the initial stage can also be described by the present model.

Stable, Microfabricated Thin Layer Chromatography Plates without Volume Distortion on Patterned, Carbon and Al2O3-Primed Carbon Nanotube Forests

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

Jensen, David S.; Kanyal, Supriya S.; Gupta, Vipul

2012-09-28

In a recent report (Song, J.; et al., Advanced Functional Materials 2011, 21, 1132-1139) some of us described the fabrication of thin layer chromatography (TLC) plates from patterned carbon nanotube (CNT) forests, which were directly infiltrated/coated with silicon by low pressure chemical vapor deposition (LPCVD) of silicon using SiH4. Following infiltration, the nanotubes were removed from the assemblies and the silicon simultaneously converted to SiO2 in a high temperature oxidation step. However, while straightforward, this process had some shortcomings, not the least of which was some distortion of the lithographically patterned features during the volume expansion that accompanied oxidation. Hereinmore » we overcome theis issue and also take substantial steps forward in the microfabrication of TLC plates by showing: (i) A new method for creating an adhesion promotion layer on CNT forests by depositing a few nanometers of carbon followed by atomic layer deposition (ALD) of Al2O3. This method for appears to be new, and X-ray photoelectron spectroscopy confirms the expected presence of oxygen after carbon deposition. ALD of Al2O3 alone and in combination with the carbon on patterned CNT forests was also explored as an adhesion promotion layer for CNT forest infiltration. (ii) Rapid, conformal deposition of an inorganic material that does not require subsequent oxidation: fast pseudo-ALD growth of SiO2 via alumina catalyzed deposition of tris(tert-butoxy)silanol onto the carbon/Al2O3-primed CNT forests. (iii) Faithful reproduction of the features in the masks used to microfabricate the TLC plates (M-TLC) this advance springs from the previous two points. (iv) A bonded (amino) phase on a CNT-templated microfabricated TLC plate. (v) Fast, highly efficient (125,000 - 225,000 N/m) separations of fluorescent dyes on M-TLC plates. (vi) Extensive characterization of our new materials by TEM, SEM, EDAX, DRIFT, and XPS. (vii) A substantially lower process temperature

Evaluation of reversed-phase nano liquid chromatography conditions by using reversed-phase thin layer chromatography based on Hansen solubility parameters for the analysis of amphiphilic glycosylsphingolipid transformations.

PubMed

Kanie, Yoshimi; Taniuchi, Mizuki; Kanie, Osamu

2018-01-26

Pulse chase analysis is often used in investigating dynamics of cellular substances. Fluorescently labeled lactosyl sphingosine molecule is useful in chasing its transformation, however the analysis of such metabolites in attomole level is of extreme difficult due to the presence of large amount of endogenous amphiphilic molecules such as glycosphingolipids, sphingomyerin, and glycerophospholipids. Nano LC suites for analyzing the attomole scale metabolites, therefore removal of endogenous substances prior to nano LC and finding appropriate nano LC conditions are necessary. Thus, we focused on the solubility of fluorescent BODIPY-labeled lactosylsphingosine (Lac-Sph-BODIPY) to identify suitable solvents to remove endogenous compounds. In this study, we evaluated solvents by using C18 thin layer chromatography (RP TLC). The mobility (R f ) of Lac-Sph-BODIPY against several solvent mixtures on RP TLC were plotted against polarity and hydrogen bonding capability followed by Hansen solubility parameters (HSPs). The optimum solvent mixture with R f  = 0.3 ± 0.1 was chosen for elimination of endogenous phospholipids on a ZrO 2 -SiO 2 cartridge column and subsequent separation by nano LC. Efficient removal of endogenous phospholipids was demonstrated, and good resolution in nano LC analysis of Lac-Sph-BODIPY extracted from Chinese hamster ovary (CHO)-K1 cells was achieved. It was also shown that the amount of exogenously added compound was important in the investigation of metabolites using cultured cells. Copyright © 2017 Elsevier B.V. All rights reserved.

Rapid Biochemical Mixture Screening by Three-Dimensional Patterned Multifunctional Substrate with Ultra-Thin Layer Chromatography (UTLC) and Surface Enhanced Raman Scattering (SERS).

PubMed

Lee, Bi-Shen; Lin, Pi-Chen; Lin, Ding-Zheng; Yen, Ta-Jen

2018-01-11

We present a three-dimensional patterned (3DP) multifunctional substrate with the functions of ultra-thin layer chromatography (UTLC) and surface enhanced Raman scattering (SERS), which simultaneously enables mixture separation, target localization and label-free detection. This multifunctional substrate is comprised of a 3DP silicon nanowires array (3DP-SiNWA), decorated with silver nano-dendrites (AgNDs) atop. The 3DP-SiNWA is fabricated by a facile photolithographic process and low-cost metal assisted chemical etching (MaCE) process. Then, the AgNDs are decorated onto 3DP-SiNWA by a wet chemical reduction process, obtaining 3DP-AgNDs@SiNWA multifunctional substrates. With various patterns designed on the substrates, the signal intensity could be maximized by the excellent confinement and concentrated effects of patterns. By using this 3DP-AgNDs@SiNWA substrate to scrutinize the mixture of two visible dyes, the individual target could be recognized and further boosted the Raman signal of target 15.42 times comparing to the un-patterned AgNDs@SiNWA substrate. Therefore, such a three-dimensional patterned multifunctional substrate empowers rapid mixture screening, and can be readily employed in practical applications for biochemical assays, food safety and other fields.

High-Performance Liquid Chromatography-Mass Spectrometry.

ERIC Educational Resources Information Center

Vestal, Marvin L.

1984-01-01

Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

Layered Organization in the Coastal Ocean: 4-D Assessment of Thin Layer Structure, Dynamics and Impacts

DTIC Science & Technology

2009-09-30

maintenance and dissipation of layers; (2) to understand the spatial coherence and spatial properties of thin layers in the coastal ocean (especially in...ORCAS profilers at K1 South and K2 had a Nortek ADV (Acoustic Doppler Velocity meter) for simultaneously measuring centimeter- scale currents and...year will be used to (1) detect the presence, intensity, thickness, temporal persistence, and spatial coherence of thin optical and acoustical layers

[In situ thin layer chromatography-fourier transform-surface-enhanced Raman spectrum study on ingredients of berberine].

PubMed

Wang, Yuan; Guo, Zhan-sheng; Wang, Ying-feng; Wang, Song-ying; Ren, Gui-fen; Zhang, Xiang-lan; Han, Xiu-lan

2002-10-01

Surface Enhanced Raman Scattering (SERS) combined with Thin Layer Chromatography (TLC) has been used for studying characteristic spectrum of molecules in situ in micrograms samples. There are very few report for applying the SERS-TCL method in the study of the effective ingredients of Chinese traditional herbs. Coptis Chinensis France is an often-used clinic Chinese traditional medicine. Its main effective components include berberine and so on, which have antibiotic very wide and also have curative effect on improving the functions of heart vascular cycles. Therefore the concentrations of berberine are very important for the quality control of the medicine. In this work, the ethanol extract of Coptis Chinensis France was first separated by TLC, the SERS was then measure directly after dropping silver gel on the separated spots. The method can be used for the finger print analysis of the berberine. 3 microL of alcohol extract of Coptis Chinensis France with total alkaloids concentration of 1.0 mg.mL was placed on silicon GF254 TLC plate. The sample was separated by developing solvent of n bulanol-Acitic acid-H2O (7:2:1 V/V). The positions of berberine in the sample were confirmed by the standard alkaloid solutions. The Rf values for berberine are 0.29. The silver gel was used as surface enhanced substrate and placed on the separated berberine spots. FT-SERS was measured directly by a Nicolet FT-Raman 910 spectrometer. Berberine belong to isoquinoline alkaloids. His structure can be found in reference. The date of spectrum of berberine can be seen that the band at 1,396 cm-1 due to Ar-OCH3 deformation vibrations was greatly enhanced, indicating that the molecule was absorbed on silver gel strongly through lone-pair electron in Ar-OCH3. The ring stretching mode occurring around 1,548 cm-1 represents isoquinoline ring in the molecule. The band at 727 cm-1 due to CH (ring) deformation vibrations was also enhanced.

Ad-hoc surface-enhanced Raman spectroscopy methodologies for the detection of artist dyestuffs: thin layer chromatography-surface enhanced Raman spectroscopy and in situ on the fiber analysis.

PubMed

Brosseau, Christa L; Gambardella, Alessa; Casadio, Francesca; Grzywacz, Cecily M; Wouters, Jan; Van Duyne, Richard P

2009-04-15

Tailored ad-hoc methods must be developed for successful identification of minute amounts of natural dyes on works of art using Surface-Enhanced Raman Spectroscopy (SERS). This article details two of these successful approaches using silver film over nanosphere (AgFON) substrates and silica gel coupled with citrate-reduced Ag colloids. The latter substrate functions as the test system for the coupling of thin-layer chromatography and SERS (TLC-SERS), which has been used in the current research to separate and characterize a mixture of several artists' dyes. The poor limit of detection of TLC is overcome by coupling with SERS, and dyes which co-elute to nearly the same spot can be distinguished from each other. In addition, in situ extractionless non-hydrolysis SERS was used to analyze dyed reference fibers, as well as historical textile fibers. Colorants such as alizarin, purpurin, carminic acid, lac dye, crocin, and Cape jasmine were thus successfully identified.

Determination of Sudan I in paprika powder by molecularly imprinted polymers-thin layer chromatography-surface enhanced Raman spectroscopic biosensor.

PubMed

Gao, Fang; Hu, Yaxi; Chen, Da; Li-Chan, Eunice C Y; Grant, Edward; Lu, Xiaonan

2015-10-01

Sudan I is a carcinogenic and mutagenic azo-compound that has been utilized as a common adulterant in spice and spice blends to impart a desirable red color to foods. A novel biosensor combining molecularly imprinted polymers (MIPs), thin layer chromatography (TLC) and surface enhanced Raman spectroscopy (SERS) could determine Sudan I levels in paprika powder to 1 ppm (or 2 ng/spot). Sudan I spiked paprika extracts (spiking levels: 0, 1, 5, 10, 40, 70 and 100 ppm) were prepared. Sudan I imprinted polymers were synthesized by employing the interaction between Sudan I (template) and methacrylic acid (functional monomer), followed by washing to remove Sudan I leaving the Sudan I-binding sites exposed. MIPs were used as a stationary phase for TLC and could selectively retain Sudan I at the original spot with little interference. A gold colloid SERS substrate could enhance Raman intensity for Sudan I in this MIP-TLC system. Principal component analysis plot and partial least squares regression (R(2)=0.978) models were constructed and a linear regression model (R(2)=0.983) correlated spiking levels (5, 10, 40, 70 and 100 ppm) with the peak intensities (721 cm(-1)) of Sudan I SERS spectra. Both separation (30-40s) and detection (1s or 0.1s) were extremely fast by using both commercial bench-top and custom made portable Raman spectrometers. This biosensor can be applied as a rapid, low-cost and reliable tool for screening Sudan I adulteration in foods. Copyright © 2015 Elsevier B.V. All rights reserved.

Advanced germanium layer transfer for ultra thin body on insulator structure

NASA Astrophysics Data System (ADS)

Maeda, Tatsuro; Chang, Wen-Hsin; Irisawa, Toshifumi; Ishii, Hiroyuki; Hattori, Hiroyuki; Poborchii, Vladimir; Kurashima, Yuuichi; Takagi, Hideki; Uchida, Noriyuki

2016-12-01

We present the HEtero-Layer Lift-Off (HELLO) technique to obtain ultra thin body (UTB) Ge on insulator (GeOI) substrates. The transferred ultra thin Ge layers are characterized by the Raman spectroscopy measurements down to the thickness of ˜1 nm, observing a strong Raman intensity enhancement for high quality GeOI structure in ultra thin regime due to quantum size effect. This advanced Ge layer transfer technique enabled us to demonstrate UTB-GeOI nMOSFETs with the body thickness of only 4 nm.

Characterization of aluminum selenide bi-layer thin film

NASA Astrophysics Data System (ADS)

Boolchandani, Sarita; Soni, Gyanesh; Srivastava, Subodh; Vijay, Y. K.

2018-05-01

The Aluminum Selenide (AlSe) bi-layer thin films were grown on glass substrate using thermal evaporation method under high vacuum condition. The morphological characterization was done using SEM. Electrical measurement with temperature variation shows that thin films exhibit the semiconductor nature. The optical properties of prepared thin films have also been characterized by UV-VIS spectroscopy measurements. The band gap of composite thin films has been calculated by Tauc's relation at different temperature ranging 35°C-100°C.

Optical characterizations of silver nanoprisms embedded in polymer thin film layers

NASA Astrophysics Data System (ADS)

Carlberg, Miriam; Pourcin, Florent; Margeat, Olivier; Le Rouzo, Judikael; Berginc, Gerard; Sauvage, Rose-Marie; Ackermann, Jorg; Escoubas, Ludovic

2017-10-01

The precise control of light-matter interaction has a wide range of applications and is currently driven by the use of nanoparticles (NPs) by the recent advances in nanotechnology. Taking advantage of the material, size, shape, and surrounding media dependence of the optical properties of plasmonic NPs, thin film layers with tunable optical properties are achieved. The NPs are synthesized by wet chemistry and embedded in a polyvinylpyrrolidone (PVP) polymer thin film layer. Spectrophotometer and spectroscopic ellipsometry measurements are coupled to finite-difference time domain numerical modeling to optically characterize the heterogeneous thin film layers. Silver nanoprisms of 10 to 50 nm edge size exhibit high absorption through the visible wavelength range. A simple optical model composed of a Cauchy law and a Lorentz law, accounting for the optical properties of the nonabsorbing polymer and the absorbing property of the nanoprisms, fits the spectroscopic ellipsometry measurements. Knowing the complex optical indices of heterogeneous thin film layers let us design layers of any optical properties.

Effects of channel thickness on oxide thin film transistor with double-stacked channel layer

NASA Astrophysics Data System (ADS)

Lee, Kimoon; Kim, Yong-Hoon; Yoon, Sung-Min; Kim, Jiwan; Oh, Min Suk

2017-11-01

To improve the field effect mobility and control the threshold voltage ( V th ) of oxide thin film transistors (TFTs), we fabricated the oxide TFTs with double-stacked channel layers which consist of thick Zn-Sn-O (ZTO) and very thin In-Zn-O (IZO) layers. We investigated the effects of the thickness of thin conductive layer and the conductivity of thick layer on oxide TFTs with doublestacked channel layer. When we changed the thickness of thin conductive IZO channel layer, the resistivity values were changed. This resistivity of thin channel layer affected on the saturation field effect mobility and the off current of TFTs. In case of the thick ZTO channel layer which was deposited by sputtering in Ar: O2 = 10: 1, the device showed better performances than that which was deposited in Ar: O2 = 1: 1. Our TFTs showed high mobility ( μ FE ) of 40.7 cm2/Vs and V th of 4.3 V. We assumed that high mobility and the controlled V th were caused by thin conductive IZO layer and thick stable ZTO layer. Therefore, this double-stacked channel structure can be very promising way to improve the electrical characteristics of various oxide thin film transistors.

Rapid and Accurate Identification of Animal Species in Natural Leather Goods by Liquid Chromatography/Mass Spectrometry

PubMed Central

Izuchi, Yukari; Takashima, Tsuneo; Hatano, Naoya

2016-01-01

The demand for leather goods has grown globally in recent years. Industry revenue is forecast to reach $91.2 billion by 2018. There is an ongoing labelling problem in the leather items market, in that it is currently impossible to identify the species that a given piece of leather is derived from. To address this issue, we developed a rapid and simple method for the specific identification of leather derived from cattle, horses, pigs, sheep, goats, and deer by analysing peptides produced by the trypsin-digestion of proteins contained in leather goods using liquid chromatography/mass spectrometry. We determined species-specific amino acid sequences by liquid chromatography/tandem mass spectrometry analysis using the Mascot software program and demonstrated that collagen α-1(I), collagen α-2(I), and collagen α-1(III) from the dermal layer of the skin are particularly useful in species identification. PMID:27313979

Fabrication of ATO/Graphene Multi-layered Transparent Conducting Thin Films

NASA Astrophysics Data System (ADS)

Li, Na; Chen, Fei; Shen, Qiang; Wang, Chuanbin; Zhang, Lianmeng

2013-03-01

A novel transparent conducting oxide based on the ATO/graphene multi-layered thin films has been developed to satisfy the application of transparent conductive electrode in solar cells. The ATO thin films are prepared by pulsed laser deposition method with high quality, namely the sheet resistance of 49.5 Ω/sq and average transmittance of 81.9 %. The prepared graphene sheet is well reduced and shows atomically thin, spotty distributed appearance on the top of the ATO thin films. The XRD and optical micrographs are used to confirm the successfully preparation of the ATO/graphene multi-layered thin films. The Hall measurements and UV-Vis spectrophotometer are conducted to evaluate the sheet resistance and optical transmittance of the innovative structure. It is found that graphene can improve the electrical properties of the ATO thin films with little influence on the optical transmittance.

Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

PubMed

Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

2016-01-01

Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The enhancement mechanism of thin plasma layer on antenna radiation

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

Wang, Chunsheng, E-mail: wangcs@hit.edu.cn; Jiang, Binhao; Li, Xueai

A model of plasma-antenna is carried out to study the radiation enhancement mechanism of antenna covered by thin plasma layer. The results show when the radiation intensity achieves maximum, a region of equal electric field is formed due to the reflection of electric field at the interface of plasma and air. The plasma layer acted as an extension of the antenna. Furthermore, the shape of plasma layer is changed to verify the effect of plasma boundary on antenna radiation. The study shows the effect of thin plasma layer on electromagnetic field and provides a type of plasma antenna.

Thin-layer voltammetry of soluble species on screen-printed electrodes: proof of concept.

PubMed

Botasini, S; Martí, A C; Méndez, E

2016-10-17

Thin-layer diffusion conditions were accomplished on screen-printed electrodes by placing a controlled-weight onto the cast solution and allowing for its natural spreading. The restricted diffusive conditions were assessed by cyclic voltammetry at low voltage scan rates and electrochemical impedance spectroscopy. The relationship between the weight exerted over the drop and the thin-layer thickness achieved was determined, in such a way that the simple experimental set-up designed for this work could be developed into a commercial device with variable control of the thin-layer conditions. The experimental results obtained resemble those reported for the voltammetric features of electroactive soluble species employing electrodes modified with carbon nanotubes or graphene layers, suggesting that the attainment of the benefits reported for these nanomaterials could be done simply by forcing the solution to spread over the screen-printed electrodic system to form a thin layer solution. The advantages of thin-layer voltammetry in the kinetic characterization of quasi-reversible and irreversible processes are highlighted.

Detecting and characterizing N-acyl-homoserine lactone signal molecules by thin-layer chromatography

PubMed Central

Shaw, Paul D.; Ping, Gao; Daly, Sean L.; Cha, Chung; Cronan, John E.; Rinehart, Kenneth L.; Farrand, Stephen K.

1997-01-01

Many Gram-negative bacteria regulate gene expression in response to their population size by sensing the level of acyl-homoserine lactone signal molecules which they produce and liberate to the environment. We have developed an assay for these signals that couples separation by thin-layer chromatography with detection using Agrobacterium tumefaciens harboring lacZ fused to a gene that is regulated by autoinduction. With the exception of N-butanoyl-l-homoserine lactone, the reporter detected acyl-homoserine lactones with 3-oxo-, 3-hydroxy-, and 3-unsubstituted side chains of all lengths tested. The intensity of the response was proportional to the amount of the signal molecule chromatographed. Each of the 3-oxo- and the 3-unsubstituted derivatives migrated with a unique mobility. Using the assay, we showed that some bacteria produce as many as five detectable signal molecules. Structures could be assigned tentatively on the basis of mobility and spot shape. The dominant species produced by Pseudomonas syringae pv. tabaci chromatographed with the properties of N-(3-oxohexanoyl)-l-homoserine lactone, a structure that was confirmed by mass spectrometry. An isolate of Pseudomonas fluorescens produced five detectable species, three of which had novel chromatographic properties. These were identified as the 3-hydroxy- forms of N-hexanoyl-, N-octanoyl-, and N-decanoyl-l-homoserine lactone. The assay can be used to screen cultures of bacteria for acyl-homoserine lactones, for quantifying the amounts of these molecules produced, and as an analytical and preparative aid in determining the structures of these signal molecules. PMID:9177164

Gravitational instability of thin gas layer between two thick liquid layers

NASA Astrophysics Data System (ADS)

Pimenova, A. V.; Goldobin, D. S.

2016-12-01

We consider the problem of gravitational instability (Rayleigh-Taylor instability) of a horizontal thin gas layer between two liquid half-spaces (or thick layers), where the light liquid overlies the heavy one. This study is motivated by the phenomenon of boiling at the surface of direct contact between two immiscible liquids, where the rate of the "break-away" of the vapor layer growing at the contact interface due to development of the Rayleigh-Taylor instability on the upper liquid-gas interface is of interest. The problem is solved analytically under the assumptions of inviscid liquids and viscous weightless vapor. These assumptions correspond well to the processes in real systems, e.g., they are relevant for the case of interfacial boiling in the system water- n-heptane. In order to verify the results, the limiting cases of infinitely thin and infinitely thick gas layers were considered, for which the results can be obviously deduced from the classical problem of the Rayleigh-Taylor instability. These limiting cases are completely identical to the well-studied cases of gravity waves at the liquidliquid and liquid-gas interfaces. When the horizontal extent of the system is long enough, the wavenumber of perturbations is not limited from below, and the system is always unstable. The wavelength of the most dangerous perturbations and the rate of their exponential growth are derived as a function of the layer thickness. The dependence of the exponential growth rate on the gas layer thickness is cubic.

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

PubMed

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.

A separable surface-enhanced Raman scattering substrate modified with MIL-101 for detection of overlapping and invisible compounds after thin-layer chromatography development.

PubMed

Zhang, Bin Bin; Shi, Yi; Chen, Hui; Zhu, Qing Xia; Lu, Feng; Li, Ying Wei

2018-01-02

By coupling surface-enhanced Raman spectroscopy (SERS) with thin-layer chromatography (TLC), a powerful method for detecting complex samples was successfully developed. However, in the TLC-SERS method, metal nanoparticles serving as the SERS-active substrate are likely to disturb the detection of target compounds, particularly in overlapping compounds after TLC development. In addition, the SERS detection of compounds that are invisible under both visible light and UV 254/365 after TLC development is still a significant challenge. In this study, we demonstrated a facile strategy to fabricate a TLC plate with metal-organic framework-modified gold nanoparticles as a separable SERS substrate, on which all separated components, including overlapping and invisible compounds, could be detected by a point-by-point SERS scan along the developing direction. Rhodamine 6G (R6G) was used as a probe to evaluate the performance of the substrate. The results indicated that the substrate provided good sensitivity and reproducibility, and optimal SERS signals could be collected in 5 s. Furthermore, this new substrate exhibited a long shelf life. Thus, our method has great potential for the sensitive and rapid detection of overlapping and invisible compounds in complex samples after TLC development. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

Identification of chemical components in Baidianling Capsule based on gas chromatography-mass spectrometry and high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry.

PubMed

Wu, Wenying; Chen, Yu; Wang, Binjie; Sun, Xiaoyang; Guo, Ping; Chen, Xiaohui

2017-08-01

Baidianling Capsule, which is made from 16 Chinese herbs, has been widely used for treating vitiligo clinically. In this study, the sensitive and rapid method has been developed for the analysis of chemical components in Baidianling Capsule by gas chromatography-mass spectrometry in combination with retention indices and high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry. Firstly, a total of 110 potential volatile compounds obtained from different extraction procedures including alkanes, alkenes, alkynes, ketones, ethers, aldehydes, alcohols, phenols, organic acids, esters, furans, pyrrole, acid amides, heterocycles, and oxides were detected from Baidianling Capsule by gas chromatography-mass spectrometry, of which 75 were identified by mass spectrometry in combination with the retention index. Then, a total of 124 components were tentatively identified by high-performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry. Fifteen constituents from Baidianling Capsule were accurately identified by comparing the retention times with those of reference compounds, others were identified by comparing the retention times and mass spectrometry data, as well as retrieving the reference literature. This study provides a practical strategy for rapidly screening and identifying the multiple constituents of a complex traditional Chinese medicine. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Liquid chromatography-mass spectrometry in metabolomics research: mass analyzers in ultra high pressure liquid chromatography coupling.

PubMed

Forcisi, Sara; Moritz, Franco; Kanawati, Basem; Tziotis, Dimitrios; Lehmann, Rainer; Schmitt-Kopplin, Philippe

2013-05-31

The present review gives an introduction into the concept of metabolomics and provides an overview of the analytical tools applied in non-targeted metabolomics with a focus on liquid chromatography (LC). LC is a powerful analytical tool in the study of complex sample matrices. A further development and configuration employing Ultra-High Pressure Liquid Chromatography (UHPLC) is optimized to provide the largest known liquid chromatographic resolution and peak capacity. Reasonably UHPLC plays an important role in separation and consequent metabolite identification of complex molecular mixtures such as bio-fluids. The most sensitive detectors for these purposes are mass spectrometers. Almost any mass analyzer can be optimized to identify and quantify small pre-defined sets of targets; however, the number of analytes in metabolomics is far greater. Optimized protocols for quantification of large sets of targets may be rendered inapplicable. Results on small target set analyses on different sample matrices are easily comparable with each other. In non-targeted metabolomics there is almost no analytical method which is applicable to all different matrices due to limitations pertaining to mass analyzers and chromatographic tools. The specifications of the most important interfaces and mass analyzers are discussed. We additionally provide an exemplary application in order to demonstrate the level of complexity which remains intractable up to date. The potential of coupling a high field Fourier Transform Ion Cyclotron Resonance Mass Spectrometer (ICR-FT/MS), the mass analyzer with the largest known mass resolving power, to UHPLC is given with an example of one human pre-treated plasma sample. This experimental example illustrates one way of overcoming the necessity of faster scanning rates in the coupling with UHPLC. The experiment enabled the extraction of thousands of features (analytical signals). A small subset of this compositional space could be mapped into a mass

Marangoni-Benard Convection in a Evaporating Liquid Thin Layer

NASA Technical Reports Server (NTRS)

Chai, An-Ti; Zhang, Nengli

1996-01-01

Marangoni-Benard convection in evaporating liquid thin layers has been investigated through flow visualization and temperature profile measurement. Twelve liquids, namely ethyl alcohol, methanol, chloroform, acetone, cyclohexane, benzine, methylene chloride, carbon tetrachloride, ethyl acetate, n-pentane, silicone oil (0.65 cSt.), and freon-113, were tested and convection patterns in thin layers of these samples were observed. Comparison among these tested samples shows that some liquids are sensitive to surface contamination from aluminum powder but some are not. The latter is excellent to be used for the investigation of surface-tension driven convection through visualization using the tracer. Two sample liquids, alcohol and freon-113 were particularly selected for systematic study. It was found that the wavelength of Benard cells would not change with thickness of the layer when it evaporates at room temperature. Special attention was focused on cases in which a liquid layer was cooled from below, and some interesting results were obtained. Convection patterns were recorded during the evaporation process and the patterns at certain time frame were compared. Benard cells were observed in thin layers with a nonlinear temperature profile and even with a zero or positive temperature gradient. Wavelength of the cells was found to increase as the evaporation progressed.

Ferroelastic switching in a layered-perovskite thin film

PubMed Central

Wang, Chuanshou; Ke, Xiaoxing; Wang, Jianjun; Liang, Renrong; Luo, Zhenlin; Tian, Yu; Yi, Di; Zhang, Qintong; Wang, Jing; Han, Xiu-Feng; Van Tendeloo, Gustaaf; Chen, Long-Qing; Nan, Ce-Wen; Ramesh, Ramamoorthy; Zhang, Jinxing

2016-01-01

A controllable ferroelastic switching in ferroelectric/multiferroic oxides is highly desirable due to the non-volatile strain and possible coupling between lattice and other order parameter in heterostructures. However, a substrate clamping usually inhibits their elastic deformation in thin films without micro/nano-patterned structure so that the integration of the non-volatile strain with thin film devices is challenging. Here, we report that reversible in-plane elastic switching with a non-volatile strain of approximately 0.4% can be achieved in layered-perovskite Bi2WO6 thin films, where the ferroelectric polarization rotates by 90° within four in-plane preferred orientations. Phase-field simulation indicates that the energy barrier of ferroelastic switching in orthorhombic Bi2WO6 film is ten times lower than the one in PbTiO3 films, revealing the origin of the switching with negligible substrate constraint. The reversible control of the in-plane strain in this layered-perovskite thin film demonstrates a new pathway to integrate mechanical deformation with nanoscale electronic and/or magnetoelectronic applications. PMID:26838483

Ferroelastic switching in a layered-perovskite thin film

DOE PAGES

Wang, Chuanshou; Ke, Xiaoxing; Wang, Jianjun; ...

2016-02-03

Here, a controllable ferroelastic switching in ferroelectric/multiferroic oxides is highly desirable due to the non-volatile strain and possible coupling between lattice and other order parameter in heterostructures. However, a substrate clamping usually inhibits their elastic deformation in thin films without micro/nano-patterned structure so that the integration of the non-volatile strain with thin film devices is challenging. Here, we report that reversible in-plane elastic switching with a non-volatile strain of approximately 0.4% can be achieved in layered-perovskite Bi 2WO 6 thin films, where the ferroelectric polarization rotates by 90° within four in-plane preferred orientations. Phase-field simulation indicates that the energy barriermore » of ferroelastic switching in orthorhombic Bi 2WO 6 film is ten times lower than the one in PbTiO 3 films, revealing the origin of the switching with negligible substrate constraint. The reversible control of the in-plane strain in this layered-perovskite thin film demonstrates a new pathway to integrate mechanical deformation with nanoscale electronic and/or magnetoelectronic applications.« less

Surface passivation investigation on ultra-thin atomic layer deposited aluminum oxide layers for their potential application to form tunnel layer passivated contacts

NASA Astrophysics Data System (ADS)

Xin, Zheng; Ling, Zhi Peng; Nandakumar, Naomi; Kaur, Gurleen; Ke, Cangming; Liao, Baochen; Aberle, Armin G.; Stangl, Rolf

2017-08-01

The surface passivation performance of atomic layer deposited ultra-thin aluminium oxide layers with different thickness in the tunnel layer regime, i.e., ranging from one atomic cycle (∼0.13 nm) to 11 atomic cycles (∼1.5 nm) on n-type silicon wafers is studied. The effect of thickness and thermal activation on passivation performance is investigated with corona-voltage metrology to measure the interface defect density D it(E) and the total interface charge Q tot. Furthermore, the bonding configuration variation of the AlO x films under various post-deposition thermal activation conditions is analyzed by Fourier transform infrared spectroscopy. Additionally, poly(3,4-ethylenedioxythiophene) poly(styrene sulfonate) is used as capping layer on ultra-thin AlO x tunneling layers to further reduce the surface recombination current density to values as low as 42 fA/cm2. This work is a useful reference for using ultra-thin ALD AlO x layers as tunnel layers in order to form hole selective passivated contacts for silicon solar cells.

Patterning layer-by-layer self-assembled multilayer by lithography and its applications to thin film devices

NASA Astrophysics Data System (ADS)

Hua, Feng

Nanoparticles are exciting materials because they exhibit unique electronic, catalytic, and optical properties. As a novel and promising nanobuilding block, it attracts considerable research efforts in its integration into a wide variety of thin film devices. Nanoparticles were adsorbed onto the substrate with layer-by-layer self-assembly which becomes of great interest due to its suitability in colloid particle assembly. Without extremely high temperatures and sophisticated equipment, molecularly organized films in an exactly pre-designed order can grow on almost all the substrates in nature. Two approaches generating spatially separated patterns comprised of nanoparticles are demonstrated, as well as two approaches patterning more than one type of nonoparticle on a silicon wafer. The structure of the thin film patterned by these approaches are analyzed and considered suitable to the thin film device. Finally, the combination of lithography and layer-by-layer (lbl) self-assembly is utilized to realize the microelectronic device with functional nonoparticles. The lbl self-assembly is the way to coat the nonoparticles and the lighography to pattern them. Based on the coating and patterning technique, a MOS-capacitor, a MOS field-effect-transistor and magnetic thin film cantilever are fabricated.

Evaluation and prevention of the negative matrix effect of terpenoids on pesticides in apples quantification by gas chromatography-tandem mass spectrometry.

PubMed

Giacinti, Géraldine; Raynaud, Christine; Capblancq, Sophie; Simon, Valérie

2016-12-21

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/MS 2 ) 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 (<0.05mgkg -1 ). A significant relationship has been found between the levels of these molecules and negative matrix effects in GC/MS 2 . 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.

Evaluation and prevention of the negative matrix effect of terpenoids on pesticides in apples quantification by gas chromatography-tandem mass spectrometry.

PubMed

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/MS 2 ) 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 (<0.05mgkg -1 ). A significant relationship has been found between the levels of these molecules and negative matrix effects in GC/MS 2 . 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.

Use of a thin-layer technique in thyroid fine needle aspiration.

PubMed

Malle, Despoina; Valeri, Rosalia-Maria; Pazaitou-Panajiotou, Kalliopi; Kiziridou, Anastasia; Vainas, Iraklis; Destouni, Charicleia

2006-01-01

To investigate the efficacy of the ThinPrep Processor (Cytyc Corporation, Boxborough, Massachusetts, U.S.A) in fine needle aspiration (FNA) of thyroid gland lesions. This study included 459 thyroid FNA specimens obtained from patients who came to our endocrinology department with various thyroid disorders over 3 years. The cytologic material was prepared using both the conventional and ThinPrep method in the first 2 years (285 cases), while in the last one only the ThinPrep method was used (1 74 cases). The smears were stained using a modified Papanicolaou procedure and May-Grünwald-Giemsa stain. Immunocytochemistry was performed on thin-layer slides using specific monoclonal antibodies when needed. Thin-layer and direct smear diagnoses were compared with the final cytologic or histologic diagnoses, when available. Our cases included 279 adenomatoid nodules, 15 cases of Hashimoto thyroiditis, 45 follicular neoplasms, 14 Hürthle cell tumors, 58 papillary carcinomas and 1 5 anaplastic carcinomas. Thin-layer preparations showed a trend toward a lower proportion of inadequate specimens and a lower false negative rate. Cytomorphologic features showed some differences between the 2 methods. Colloid was less frequently observed on ThinPrep slides, while nuclear detail and micronucleoli were more easily detected with this technique. Moreover, ThinPrep appeared to be the appropriate method for the use of ancillary techniques in suspicious cases. Thin-layer cytology improves the diagnostic accuracy of thyroid FNA and offers the possibility of performing new techniques, such as immunocytochemistry, on the same sample in order to detect malignancy as well as the type and origin of thyroid gland neoplasms.

Thin Carbon Layers on Nanostructured Silicon-Properties and Applications

NASA Astrophysics Data System (ADS)

Angelescu, Anca; Kleps, Irina; Miu, Mihaela; Simion, Monica; Bragaru, Adina; Petrescu, Stefana; Paduraru, Crina; Raducanu, Aurelia

Thin carbon layers such as silicon carbide (SiC) and diamond like carbon (DLC) layers on silicon, or on nanostructured silicon substrats were obtained by different methods. This paper is a review of our results in the areas of carbon layer microfabrication technologies and their properties related to different microsystem apllications. So, silicon membranes using a-SiC or DLC layers as etching mask, as well as silicon carbide membranes using a combined porous silicon — DLC structure were fabricated for sensor applications. A detailed evaluation of the field emission (FE) properties of these films was done to demonstrate their capability to be used in field emission devices. Carbon thin layers on nanostructured silicon samples were also investigated with respect to the living cell adhesion on these structures. The experiments indicate that the cell attachment on the surface of carbon coatings can be controlled by deposition parameters during the technological process.

Evaluation of Caesalpinia bonducella flower extract for anti-inflammatory action in rats and its high performance thin layer chromatography chemical fingerprinting.

PubMed

Arunadevi, Rathinam; Murugammal, Shanmugam; Kumar, Dinesh; Tandan, Surendra Kumar

2015-01-01

The study is aimed to evaluate anti-inflammatory activity of Caesalpinia bonducella Fleming (Caesalpiniaceae) flower extract (CBFE) and to study its effect on radiographic outcome in adjuvant induced arthritis and authentication by high performance thin layer chromatography (HPTLC) chemical fingerprinting. CBFE was administered orally (30, 100, and 300 mg/kg b.wt.) and tested for its anti-inflammatory activity in carrageenan-induced inflammation, cotton pellet induced chronic granulomatous inflammation and autacoids-induced inflammation. Effect on radiographic outcome was tested in adjuvant-induced arthritis. CBFE was HPTLC fingerprinted in suitable solvent system. In carrageenan-induced inflammation, CBFE produced significant inhibition in edema volume at all the doses (30, 100 and 300 mg/kg b.wt.) and percentage of inhibition was 28.68, 31.00, and 22.48, respectively as compared to control at 5 h of its administration. In cotton pellet granuloma assay, CBFE significantly decreased the granuloma weight at 300 mg/kg dose level by 22.53%. CBFE (300 mg/kg) caused significant inhibition by 37.5, 44.44, and 35.29% edema volume, at ½, 1 and 3 h after 5-hydroxytryptamine injection, respectively. Radiographic score of animals treated with 300 mg/kg CBFE was significantly decreased when compared to arthritic control animals. The extract was found to possess significant anti-inflammatory activity. CBFE treatment improved the bony architecture in adjuvant-induced arthritis in rats. The developed HPTLC fingerprint would be helpful in the authentication of C. bonducella flower extract.

Facile on-site detection of substituted aromatic pollutants in water using thin layer chromatography combined with surface-enhanced Raman spectroscopy.

PubMed

Li, Dawei; Qu, Lulu; Zhai, Wenlei; Xue, Jinqun; Fossey, John S; Long, Yitao

2011-05-01

A novel facile method for on-site detection of substituted aromatic pollutants in water using thin layer chromatography (TLC) combined with surface-enhanced Raman spectroscopy (SERS) was explored. Various substituted aromatics in polluted water were separated by a convenient TLC protocol and then detected using a portable Raman spectrometer with the prepared silver colloids serving as SERS-active substrates. The effects of operating conditions on detection efficacy were evaluated, and the application of TLC-SERS to on-site detection of artificial and real-life samples of aromatics/polluted water was systematically investigated. It was shown that commercially available Si 60-F(254) TLC plates were suitable for separation and displayed low SERS background and good separation efficiency, 2 mM silver colloids, 20 mM NaCl (working as aggregating agent), 40 mW laser power, and 50 s intergration time were appropriate for the detection regime. Furthermore, qualitative and quantitative detection of most of substituted aromatic pollutants was found to be readily accomplished using the developed TLC-SERS technique, which compared well with GC-MS in terms of identification ability and detection accuracy, and a limit of detection (LOD) less than 0.2 ppm (even at ppb level for some analytes) could be achieved under optimal conditions. The results reveal that the presented convenient method could be used for the effective separation and detection of the substituted aromatic pollutants of water on site, thus reducing possible influences of sample transportation and contamination while shortening the overall analysis time for emergency and routine monitoring of the substituted aromatics/polluted water.

Photoluminescence-based quality control for thin film absorber layers of photovoltaic devices

DOEpatents

Repins, Ingrid L.; Kuciauskas, Darius

2015-07-07

A time-resolved photoluminescence-based system providing quality control during manufacture of thin film absorber layers for photovoltaic devices. The system includes a laser generating excitation beams and an optical fiber with an end used both for directing each excitation beam onto a thin film absorber layer and for collecting photoluminescence from the absorber layer. The system includes a processor determining a quality control parameter such as minority carrier lifetime of the thin film absorber layer based on the collected photoluminescence. In some implementations, the laser is a low power, pulsed diode laser having photon energy at least great enough to excite electron hole pairs in the thin film absorber layer. The scattered light may be filterable from the collected photoluminescence, and the system may include a dichroic beam splitter and a filter that transmit the photoluminescence and remove scattered laser light prior to delivery to a photodetector and a digital oscilloscope.

Thin-Film Power Transformers

NASA Technical Reports Server (NTRS)

Katti, Romney R.

1995-01-01

Transformer core made of thin layers of insulating material interspersed with thin layers of ferromagnetic material. Flux-linking conductors made of thinner nonferromagnetic-conductor/insulator multilayers wrapped around core. Transformers have geometric features finer than those of transformers made in customary way by machining and mechanical pressing. In addition, some thin-film materials exhibit magnetic-flux-carrying capabilities superior to those of customary bulk transformer materials. Suitable for low-cost, high-yield mass production.

Nevoid melanoma of the vagina: report of one case diagnosed on thin layer cytological preparations.

PubMed

Fulciniti, Franco; Ascierto, Paolo Antonio; Simeone, Ester; Bove, Patrizia; Losito, Simona; Russo, Serena; Gallo, Maria Stella; Greggi, Stefano

2007-07-03

Primary melanoma of the vagina is an extremely rare neoplasm with approximately 250 reported cases in the world literature 1234. In its amelanotic variant this lesion may raise several differential diagnostic problems in cytological specimens 5. In this setting, the usage of thin layer cytopathological techniques (Liquid Based Preparations = LBP) may enhance the diagnostic sensitivity by permitting immunocytochemical study without having to repeat the sampling procedure. The aim of this paper is to describe the cytomorphological presentation of primary vaginal melanoma on LBP since it has not previously been reported up to now, to our knowledge. a 79-y-o female complaining of vulvar itching and yellowish vaginal discharge underwent a complete gynaecological evaluation during which a LBP cytological sample was taken from a suspicious whitish mass protruding into the vaginal lumen. A cytopathological diagnosis of amelanotic melanoma was rendered. The mass was radically excised and the patient was treated with alpha-Interferon. amelanotic melanoma may be successfully diagnosed on LBP cytological preparations. Thin layer preparations may enhance the diagnostic cytomorphological clues to its diagnosis and may permit an adequate immunocytochemical characterization of the neoplasm.

Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

PubMed

Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

2016-09-01

In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

MICELLAR ELECTROKINETIC CHROMATOGRAPHY-MASS SPECTROMETRY (R823292)

EPA Science Inventory

The combination of micellar electrokinetic chromatography (MEKC) with mass spectrometry (MS) is very attractive for the direct identification of analyte molecules, for the possibility of selectivity enhancement, and for the structure confirmation and analysis in a MS-MS mode. The...

Formation of a highly doped ultra-thin amorphous carbon layer by ion bombardment of graphene.

PubMed

Michałowski, Paweł Piotr; Pasternak, Iwona; Ciepielewski, Paweł; Guinea, Francisco; Strupiński, Włodek

2018-07-27

Ion bombardment of graphene leads to the formation of defects which may be used to tune properties of the graphene based devices. In this work, however, we present that the presence of the graphene layer on a surface of a sample has a significant impact on the ion bombardment process: broken sp 2 bonds react with the incoming ions and trap them close to the surface of the sample, preventing a standard ion implantation. For an ion bombardment with a low impact energy and significant dose (in the range of 10 14 atoms cm -2 ) an amorphization of the graphene layer is observed but at the same time, most of the incoming ions do not penetrate the sample but stop at the surface, thus forming a highly doped ultra-thin amorphous carbon layer. The effect may be used to create thin layers containing desired atoms if no other technique is available. This approach is particularly useful for secondary ion mass spectrometry where a high concentration of Cs at the surface of a sample significantly enhances the negative ionization probability, allowing it to reach better detection limits.

Formation of a highly doped ultra-thin amorphous carbon layer by ion bombardment of graphene

NASA Astrophysics Data System (ADS)

Piotr Michałowski, Paweł; Pasternak, Iwona; Ciepielewski, Paweł; Guinea, Francisco; Strupiński, Włodek

2018-07-01

Ion bombardment of graphene leads to the formation of defects which may be used to tune properties of the graphene based devices. In this work, however, we present that the presence of the graphene layer on a surface of a sample has a significant impact on the ion bombardment process: broken sp2 bonds react with the incoming ions and trap them close to the surface of the sample, preventing a standard ion implantation. For an ion bombardment with a low impact energy and significant dose (in the range of 1014 atoms cm‑2) an amorphization of the graphene layer is observed but at the same time, most of the incoming ions do not penetrate the sample but stop at the surface, thus forming a highly doped ultra-thin amorphous carbon layer. The effect may be used to create thin layers containing desired atoms if no other technique is available. This approach is particularly useful for secondary ion mass spectrometry where a high concentration of Cs at the surface of a sample significantly enhances the negative ionization probability, allowing it to reach better detection limits.

Structural analysis of commercial ceramides by gas chromatography-mass spectrometry.

PubMed

Bleton, J; Gaudin, K; Chaminade, P; Goursaud, S; Baillet, A; Tchapla, A

2001-05-11

A simple method using gas chromatography-mass spectrometry was applied to analyse structures of ceramides. Identification of trimethylsilylated ceramides were obtained in short analysis times (derivatization of ceramides in 30 min at room temperature and 20 min gas chromatography mass spectrometry run) even for complex mixtures. For example in ceramide Type III, 18 peaks were observed which represent 27 various structures. The coeluted compounds were ceramides containing the same functional groups and the same carbon number but with a different distribution on the two alkyl chains of the molecule. They were accurately differentiated by mass spectrometry. Therefore, 83 structures of trimethylsilylated ceramides were identified in 11 different commercial mixtures. For 52 structures of these, mass spectral data were not described in the literature, neither full mass spectra nor characteristic fragments.

Analysis of triterpenoids and phytosterols in vegetables by thin-layer chromatography coupled to tandem mass spectrometry.

PubMed

Naumoska, Katerina; Vovk, Irena

2015-02-13

Three TLC methods were used for an initial screening of some common plant triterpenoids and phytosterols in cuticular wax extracts of different vegetables (zucchini, eggplant, tomato, red pepper, mangold, spinach, lettuce, white-colored radicchio di Castelfranco, raddichio Leonardo, white cabbage, red cabbage and savoy cabbage). The preliminary experiments showed that the studied vegetables are potential sources of triterpenoids and phytosterols. To identify the compounds present in the extracts with high certainty, the first TLC-MS(2) method was developed for the analysis of eight triterpenoids (lupeol, α-amyrin, β-amyrin, cycloartenol, cycloartenol acetate, lupeol acetate, lupenone and friedelin) and two phytosterols (β-sitosterol and stigmasterol). This method takes the advantages of: (1) a satisfactory separation of the target compounds; (2) their differentiation according to the band colors; and (3) the potential of their discrimination by the acquired first-order mass (MS) and product ion (MS(2)) spectra. Since the closely eluting compounds have complex and similar MS(2) spectra, distinguishing between them was possible by the proposed characteristic ions. Using a custom-built mass spectral library, the head to tail MS(2) spectra comparison of sample test solution zones and standard aided the compound identification. In addition to the molecular mass information, the developed atmospheric pressure chemical ionization method (APCI) in positive ion mode provided structural information, regarding the presence of functional group in the molecule. This approach resulted in many positively assigned compounds in the investigated vegetable waxes, from which more than a half are reported for the first time. Copyright © 2015 Elsevier B.V. All rights reserved.

Critical Transitions in Thin Layer Turbulence

NASA Astrophysics Data System (ADS)

Benavides, Santiago; Alexakis, Alexandros

2017-11-01

We investigate a model of thin layer turbulence that follows the evolution of the two-dimensional motions u2 D (x , y) along the horizontal directions (x , y) coupled to a single Fourier mode along the vertical direction (z) of the form uq (x , y , z) = [vx (x , y) sin (qz) ,vy (x , y) sin (qz) ,vz (x , y) cos (qz) ] , reducing thus the system to two coupled, two-dimensional equations. Its reduced dimensionality allows a thorough investigation of the transition from a forward to an inverse cascade of energy as the thickness of the layer H = π / q is varied.Starting from a thick layer and reducing its thickness it is shown that two critical heights are met (i) one for which the forward unidirectional cascade (similar to three-dimensional turbulence) transitions to a bidirectional cascade transferring energy to both small and large scales and (ii) one for which the bidirectional cascade transitions to a unidirectional inverse cascade when the layer becomes very thin (similar to two-dimensional turbulence). The two critical heights are shown to have different properties close to criticality that we are able to analyze with numerical simulations for a wide range of Reynolds numbers and aspect ratios. This work was Granted access to the HPC resources of MesoPSL financed by the Region Ile de France and the project Equip@Meso (reference ANR-10-EQPX-29-01).

A One-Pot Synthesis of m-Terphenyls: A Guided Exploration of Reaction Chemistry, Chromatography, and Spectroscopy. A Miniproject for the Advanced Organic Chemistry Laboratory

NASA Astrophysics Data System (ADS)

Anam, Kishorekumar T.; Curtis, Michael P.; Irfan, Muhammad J.; Johnson, Michael P.; Royer, Andrew P.; Shahmohammadi, Kianor; Vinod, Thottumkara K.

2002-05-01

This four-week project-based laboratory exercise, developed for advanced organic chemistry students, involves a one-pot synthesis of m-terphenyls. Chemistry of aryl diazonium salts and Grignard reagents and reactivity of aryne intermediates toward nucleophilic reagents form the reaction chemistry basis for the project. The project exposes students to a number of important laboratory techniques (thin-layer chromatography, gas chromatography-mass spectrometry, and column chromatography) for monitoring reaction progress and product isolation. A variety of spectroscopic techniques, including IR, 1H NMR, 13C NMR, and attached proton test are used for product characterization. Students are also introduced to a useful empirical relationship to help predict (with considerable accuracy) the 13C chemical shift values of carbon atoms of substituted benzenes.

Effect of thin oxide layers incorporated in spin valve structures

NASA Astrophysics Data System (ADS)

Gillies, M. F.; Kuiper, A. E. T.; Leibbrandt, G. W. R.

2001-06-01

The enhancement of the magnetoresistance effect, induced by incorporating nano-oxide layers (NOLs) in a bottom-type spin valve, was studied for various preparation conditions. The effect of a NOL in the Co90Fe10 pinned layer was found to depend critically on the oxygen pressure applied to form the thin oxide film. Pressures over 10-3 Torr O2 yield oxides thicker than about 0.7 nm, which apparently deteriorate the biasing field which exists over the oxide. The magnetoresistance values can further be raised by forming a specular reflecting oxide on top of the sense layer. Promising results were obtained with an Al2O3 capping layer formed in a solid-state oxidation reaction that occurs spontaneously when a thin Al layer is deposited on the oxidized surface of the Co90Fe10 sense layer.

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

NASA Astrophysics Data System (ADS)

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.

Forensic applications of supercritical fluid chromatography - mass spectrometry.

PubMed

Pauk, Volodymyr; Lemr, Karel

2018-06-01

Achievements of supercritical fluid chromatography with mass spectrometric detection made in the field of forensic science during the last decade are reviewed. The main topics include analysis of traditional drugs of abuse (e.g. cannabis, methamphetamine) as well as new psychoactive substances (synthetic cannabinoids, cathinones and phenethylamines), doping agents (anabolic steroids, stimulants, diuretics, analgesics etc.) and chemical warfare agents. Control of food authenticity, detection of adulteration and identification of toxic substances in food are also pointed out. Main aspects of an analytical workflow, such as sample preparation, separation and detection are discussed. A special attention is paid to the performance characteristics and validation parameters of supercritical fluid chromatography-mass spectrometric methods in comparison with other separation techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

Fermi level de-pinning of aluminium contacts to n-type germanium using thin atomic layer deposited layers

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

Gajula, D. R., E-mail: dgajula01@qub.ac.uk; Baine, P.; Armstrong, B. M.

Fermi-level pinning of aluminium on n-type germanium (n-Ge) was reduced by insertion of a thin interfacial dielectric by atomic layer deposition. The barrier height for aluminium contacts on n-Ge was reduced from 0.7 eV to a value of 0.28 eV for a thin Al{sub 2}O{sub 3} interfacial layer (∼2.8 nm). For diodes with an Al{sub 2}O{sub 3} interfacial layer, the contact resistance started to increase for layer thicknesses above 2.8 nm. For diodes with a HfO{sub 2} interfacial layer, the barrier height was also reduced but the contact resistance increased dramatically for layer thicknesses above 1.5 nm.

"Dry-column" chromatography of plant pigments

NASA Technical Reports Server (NTRS)

Woeller, F. H.; Lehwalt, M. F.; Oyama, V. I.

1973-01-01

Separation of plant pigments which can be accomplished on thin-layer silica plates with mixture of petroleum ether, halocarbon, acetone, and polar solvent can be readily translated into dry-column technique that yields reproducible chromatograms after elution in fashion of liquid chromatography with fluorimeter as detector. Best solvent system was found to be mixture of petroleum ether, dichloromethane, acetone, and ethyl acetate.

Thin-layer chromatographic separation of conjugates of ursodeoxycholic acid from those of litho-, chenodeoxy-, deoxy-, and cholic acids.

PubMed

Batta, A K; Shefer, S; Salen, G

1981-05-01

Separation of the glycine and taurine conjugates of ursodeoxycholic acid from those of lithocholic acid, chenodeoxycholic acid, deoxycholic acid, and cholic acid by thin-layer chromatography is described. Thus, on running a silica gel G plate first in a solvent system of n-butanol-water 20:3 and then in a second solvent system of chloroform-isopropanol-acetic acid-water 30:20:4:1, all the above-mentioned conjugated bile acids are separated from one another. The application of this method to study the change in the biliary bile acid conjugation pattern in ursodeoxycholic acid-fed gallstone patients is described.

Profiling of patterned metal layers by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)

NASA Astrophysics Data System (ADS)

Bi, Melody; Ruiz, Antonio M.; Gornushkin, Igor; Smith, Ben W.; Winefordner, James D.

2000-02-01

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was used for profiling patterned thin metal layers on a polymer/silicon substrate. The parameters of the laser and ICP-MS operating conditions have been studied and optimized for this purpose. A new laser ablation chamber was designed and built to achieve the best spatial resolution. The results of the profiling by LA-ICP-MS were compared to those obtained from a laser ablation optical emission spectrometry (LA-OES) instrument, which measured the emission of the plasma at the sample surface, and thus, eliminated the time delay caused by the sample transport into the ICP-MS system. Emission spectra gave better spatial resolution than mass spectra. However, LA-ICP-MS provided much better sensitivity and was able to profile thin metal layers (on the order of a few nanometers) on the silicon surface. A lateral spatial resolution of 45 μm was achieved.

Planar chromatography mediated screening of tetracycline and fluoroquinolone antibiotics in milk by fluorescence and mass selective detection.

PubMed

Chen, Yisheng; Schwack, Wolfgang

2013-10-18

A rapid and efficient method for preliminary screening of four tetracyclines (tetracycline, chlortetracycline, oxytetracycline, doxycline) and three fluoroquinolones (enrofloxacin, ciprofloxacin, marbofloxacin), mostly detected in milk, by high-performance thin-layer chromatography-fluorescence detection and electrospray ionization mass spectrometry (HPTLC-FLD-ESI/MS) is highlighted. The optimized separation of the target antibiotics on ethylenediamine tetraacetic acid modified silica gel plates showed marked benefits for screening purposes. Besides, selective and sensitive densitometry in fluorescence mode was established with excitation at 366nm for the tetracyclines, 300nm for enrofloxacin and ciprofloxacin, and 280nm for marbofloxacin. Limits of detection (LOD) and quantitation (LOQ) with 95% confidence were in the range of 12-25 and 45-95μg/kg, respectively, in milk samples. Recoveries of target antibiotics from milk samples spiked at three critical levels (50, 100 and 150μg/kg) ranged from 76% to 105%. More importantly, a mass selective detection (MSD) was established as additional tool for confirmatory purposes. Using the elution-head based TLC-MS interface, the optimized elution flow consisting of acetonitrile/ammonium formate buffer (9/1, v/v) at a rate of 0.3mL/min enabled time-dependent resolution of analytes from the major interfering compounds, thus circumventing serious ion suppression effects. The established MSD assay also offered high sensitivity (25μg/kg) for confirmation, meeting Commission Regulation (EU) No. 37/2010. Copyright © 2013 Elsevier B.V. All rights reserved.

Detection of structurally similar adulterants in botanical dietary supplements by thin-layer chromatography and surface enhanced Raman spectroscopy combined with two-dimensional correlation spectroscopy.

PubMed

Li, Hao; Zhu, Qing xia; Chwee, Tsz sian; Wu, Lin; Chai, Yi feng; Lu, Feng; Yuan, Yong fang

2015-07-09

Thin-layer chromatography (TLC) coupled with surface enhanced Raman spectroscopy (SERS) has been widely used for the study of various complex systems, especially for the detection of adulterants in botanical dietary supplements (BDS). However, this method is not sufficient to distinguish structurally similar adulterants in BDS since the analogs have highly similar chromatographic and/or spectroscopic behaviors. Taking into account the fact that higher cost and more time will be required for comprehensive chromatographic separation, more efforts with respect to spectroscopy are now focused on analyzing the overlapped SERS peaks. In this paper, the combination of a TLC-SERS method with two-dimensional correlation spectroscopy (2DCOS), with duration of exposure to laser as the perturbation, is applied to solve this problem. Besides the usual advantages of the TLC-SERS method, such as its simplicity, rapidness, and sensitivity, more advantages are presented here, such as enhanced selectivity and good reproducibility, which are obtained by 2DCOS. Two chemicals with similar structures are successfully differentiated from the complex BDS matrices. The study provides a more accurate qualitative screening method for detection of BDS with adulterants, and offers a new universal approach for the analysis of highly overlapped SERS peaks. Copyright © 2015 Elsevier B.V. All rights reserved.

A comprehensive review of thin-layer drying models used in agricultural products.

PubMed

Ertekin, Can; Firat, M Ziya

2017-03-04

Drying is one of the widely used methods of grain, fruit, and vegetable preservation. The important aim of drying is to reduce the moisture content and thereby increase the lifetime of products by limiting enzymatic and oxidative degradation. In addition, by reducing the amount of water, drying reduces the crop losses, improves the quality of dried products, and facilitates its transportation, handling, and storage requirements. Drying is a process comprising simultaneous heat and mass transfer within the material, and between the surface of the material and the surrounding media. Many models have been used to describe the drying process for different agricultural products. These models are used to estimate drying time of several products under different drying conditions, and how to increase the drying process efficiency and also to generalize drying curves, for the design and operation of dryers. Several investigators have proposed numerous mathematical models for thin-layer drying of many agricultural products. This study gives a comprehensive review of more than 100 different semitheoretical and empirical thin-layer drying models used in agricultural products and evaluates the statistical criteria for the determination of appropriate model.

Layered Organization in the Coastal Ocean: 4-D Assessment of Thin Layer Structure, Dynamics and Impacts

DTIC Science & Technology

2007-09-30

For example, the differences seen between the waters off of the US Pacific Northwest and the California Bight are almost certainly a reflection of the...the Pacific Northwest were favorable for thin layer development during that study. This is even more evident in those cases where thin layers...approach during the 2005 and 2006 LOCO process study combined time series data from an array of our Ocean Response Coastal Analysis System ( ORCAS ) (Donaghay

Uniaxially aligned electrospun cellulose acetate nanofibers for thin layer chromatographic screening of hydroquinone and retinoic acid adulterated in cosmetics.

PubMed

Tidjarat, Siripran; Winotapun, Weerapath; Opanasopit, Praneet; Ngawhirunpat, Tanasait; Rojanarata, Theerasak

2014-11-07

Uniaxially aligned cellulose acetate (CA) nanofibers were successfully fabricated by electrospinning and applied to use as stationary phase for thin layer chromatography. The control of alignment was achieved by using a drum collector rotating at a high speed of 6000 rpm. Spin time of 6h was used to produce the fiber thickness of about 10 μm which was adequate for good separation. Without any chemical modification after the electrospinning process, CA nanofibers could be readily devised for screening hydroquinone (HQ) and retinoic acid (RA) adulterated in cosmetics using the mobile phase consisting of 65:35:2.5 methanol/water/acetic acid. It was found that the separation run on the aligned nanofibers over a distance of 5 cm took less than 15 min which was two to three times faster than that on the non-aligned ones. On the aligned nanofibers, the masses of HQ and RA which could be visualized were 10 and 25 ng, respectively, which were two times lower than those on the non-aligned CA fibers and five times lower than those on conventional silica plates due to the appearance of darker and sharper of spots on the aligned nanofibers. Furthermore, the proposed method efficiently resolved HQ from RA and ingredients commonly found in cosmetic creams. Due to the satisfactory analytical performance, facile and inexpensive production process, uniaxially aligned electrospun CA nanofibers are promising alternative media for planar chromatography. Copyright © 2014 Elsevier B.V. All rights reserved.

Thin Layer Drying Model of Bacterial Cellulose Film

NASA Astrophysics Data System (ADS)

Hadi Jatmiko, Tri; Taufika Rosyida, Vita; Wheni Indrianingsih, Anastasia; Apriyana, Wuri

2017-12-01

The bacterial cellulose film produced by Acetobacter xylinum using coconut water as a carbon source was dried at a temperature of 60 to 100 C. The drying process of bacterial cellulose film occur at falling rate drying period. Increasing drying temperature will shorten the drying time. The drying data fitted with thin layer drying models that widely used, Newton, Page and Henderson and Pabis models. All thin layer drying models describe the experimental data well, but Page model is better than the other models on all various temperature with coefficients of determination (R2) range from 0.9908 to 0.9979, chi square range from 0.000212 to 0.000851 and RMSE range from 0.014307 to 0.0289458.

Electrochemical Atomic Layer Epitaxy of Thin Film CdSe

NASA Astrophysics Data System (ADS)

Pham, L.; Kaleida, K.; Happek, U.; Mathe, M. K.; Vaidyanathan, R.; Stickney, J. L.; Radevic, M.

2002-10-01

Electrochemical atomic layer epitaxy (EC-ALE) is a current developmental technique for the fabrication of compound semiconductor thin films. The deposition of elements making up the compound utilizes surface limited reactions where the potential is less than that required for bulk growth. This growth method offers mono-atomic layer control, allowing the deposition of superlattices with sharp interfaces. Here we report on the EC-ALE formation of CdSe thin films on Au and Cu substrates using an automated flow cell system. The band gap was measured using IR absorption and photoconductivity and found to be consistent with the literature value of 1.74 eV at 300K and 1.85 eV at 20K. The stoichiometry of the thin film was confirmed with electron microprobe analysis and x-ray diffraction.

Influences of Indium Tin Oxide Layer on the Properties of RF Magnetron-Sputtered (BaSr)TiO3 Thin Films on Indium Tin Oxide-Coated Glass Substrate

NASA Astrophysics Data System (ADS)

Kim, Tae Song; Oh, Myung Hwan; Kim, Chong Hee

1993-06-01

Nearly stoichiometric ((Ba+Sr)/Ti=1.08-1.09) and optically transparent (BaSr)TiO3 thin films were deposited on an indium tin oxide (ITO)-coated glass substrate by means of rf magnetron sputtering for their application to the insulating layer of an electroluminescent flat panel display. The influence of the ITO layer on the properties of (BaSr)TiO3 thin films deposited on the ITO-coated substrate was investigated. The ITO layer did not affect the crystallographic orientation of (BaSr)TiO3 thin film, but enhanced the grain growth. Another effect of the ITO layer on (BaSr)TiO3 thin films was the interdiffusion phenomenon, which was studied by means of secondary ion mass spectrometry (SIMS). As the substrate temperature increased, interdiffusion intensified at the interface not only between the grown film and ITO layer but also between the ITO layer and base glass substrate. The refractive index (nf) of (BaSr)TiO3 thin film deposited on a bare glass substrate was 2.138-2.286, as a function of substrate temperature.

Characterization of Cu buffer layers for growth of L10-FeNi thin films

NASA Astrophysics Data System (ADS)

Mizuguchi, M.; Sekiya, S.; Takanashi, K.

2010-05-01

A Cu(001) layer was fabricated on a Au(001) layer to investigate the use of Cu as a buffer layer for growing L10-FeNi thin films. The epitaxial growth of a Cu buffer layer was observed using reflection high-energy electron diffraction. The flatness of the layer improved drastically with an increase in the substrate temperature although the layer was an alloy (AuCu3). An FeNi thin film was epitaxially grown on the AuCu3 buffer layer by alternate monatomic layer deposition and the formation of an L10-FeNi ordered alloy was expected. The AuCu3 buffer layer is thus a promising candidate material for the growth of L10-FeNi thin films.

Mass-spring matching layers for high-frequency ultrasound transducers: a new technique using vacuum deposition.

PubMed

Brown, Jeremy; Sharma, Srikanta; Leadbetter, Jeff; Cochran, Sandy; Adamson, Rob

2014-11-01

We have developed a technique of applying multiple matching layers to high-frequency (>30 MHz) imaging transducers, by using carefully controlled vacuum deposition alone. This technique uses a thin mass-spring matching layer approach that was previously described in a low-frequency (1 to 10 MHz) transducer design with epoxied layers. This mass- spring approach is more suitable to vacuum deposition in highfrequency transducers over the conventional quarter-wavelength resonant cavity approach, because thinner layers and more versatile material selection can be used, the difficulty in precisely lapping quarter-wavelength matching layers is avoided, the layers are less attenuating, and the layers can be applied to a curved surface. Two different 3-mm-diameter 45-MHz planar lithium niobate transducers and one geometrically curved 3-mm lithium niobate transducer were designed and fabricated using this matching layer approach with copper as the mass layer and parylene as the spring layer. The first planar lithium niobate transducer used a single mass-spring matching network, and the second planar lithium niobate transducer used a single mass-spring network to approximate the first layer in a dual quarter-wavelength matching layer system in addition to a conventional quarter-wavelength layer as the second matching layer. The curved lithium niobate transducer was press focused and used a similar mass-spring plus quarter-wavelength matching layer network. These transducers were then compared with identical transducers with no matching layers and the performance improvement was quantified. The bandwidth of the lithium niobate transducer with the single mass-spring layer was measured to be 46% and the insertion loss was measured to be -21.9 dB. The bandwidth and insertion loss of the lithium niobate transducer with the mass-spring network plus quarter-wavelength matching were measured to be 59% and -18.2 dB, respectively. These values were compared with the unmatched

Polymer thin film as coating layer to prevent corrosion of metal/metal oxide film

NASA Astrophysics Data System (ADS)

Sarkar, Suman; Kundu, Sarathi

2018-04-01

Thin film of polymer is used as coating layer and the corrosion of metal/metal oxide layer is studied with the variation of the thickness of the coating layer. The thin layer of polystyrene is fabricated using spin coating method on copper oxide (CuO) film which is deposited on glass substrate using DC magnetron sputtering technique. Thickness of the polystyrene and the CuO layers are determined using X-ray reflectivity (XRR) technique. CuO thin films coated with the polystyrene layer are exposed to acetic acid (2.5 v/v% aqueous CH3COOH solution) environments and are subsequently analyzed using UV-Vis spectroscopy and atomic force microscopy (AFM). Surface morphology of the film before and after interaction with the acidic environment is determined using AFM. Results obtained from the XRR and UV-Vis spectroscopy confirm that the thin film of polystyrene acts as an anticorrosion coating layer and the strength of the coating depends upon the polymer layer thickness at a constant acid concentration.

Fabrication of Organic Thin Film Transistors Using Layer-By-Layer Assembly (Preprint)

DTIC Science & Technology

2007-03-01

thin-film transistors ( TFTs ) have received considerable attention as a low- cost, light-weight, flexible alternative to traditional amorphous silicon...Previous studies have investigated the use of a number of materials for both the active layer and the gate dielectric in various TFT architectures. These...performance. Conjugated small molecules, such as pentacene, or polymers, such as poly(3- hexylthiophene), are commonly used as the active layer in organic TFT

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

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

Nurhandoko, Bagus Endar B., E-mail: bagusnur@bdg.centrin.net.id, E-mail: bagusnur@rock-fluid.com; Rock Fluid Imaging Lab., Bandung; Susilowati, E-mail: bagusnur@bdg.centrin.net.id, E-mail: bagusnur@rock-fluid.com

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 aboutmore » 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.« less

Thin layer chromatography-densitometric determination of some non-sedating antihistamines in combination with pseudoephedrine or acetaminophen in synthetic mixtures and in pharmaceutical formulations.

PubMed

El-Kommos, Michael E; El-Gizawy, Samia M; Atia, Noha N; Hosny, Noha M

2014-03-01

The combination of certain non-sedating antihistamines (NSA) such as fexofenadine (FXD), ketotifen (KET) and loratadine (LOR) with pseudoephedrine (PSE) or acetaminophen (ACE) is widely used in the treatment of allergic rhinitis, conjunctivitis and chronic urticaria. A rapid, simple, selective and precise densitometric method was developed and validated for simultaneous estimation of six synthetic binary mixtures and their pharmaceutical dosage forms. The method employed thin layer chromatography aluminum plates precoated with silica gel G 60 F254 as the stationary phase. The mobile phases chosen for development gave compact bands for the mixtures FXD-PSE (I), KET-PSE (II), LOR-PSE (III), FXD-ACE (IV), KET-ACE (V) and LOR-ACE (VI) [Retardation factor (Rf ) values were (0.20, 0.32), (0.69, 0.34), (0.79, 0.13), (0.36, 0.70), (0.51, 0.30) and (0.76, 0.26), respectively]. Spectrodensitometric scanning integration was performed at 217, 218, 218, 233, 272 and 251 nm for the mixtures I-VI, respectively. The linear regression data for the calibration plots showed an excellent linear relationship. The method was validated for precision, accuracy, robustness and recovery. Limits of detection and quantitation were calculated. Statistical analysis proved that the method is reproducible and selective for the simultaneous estimation of these binary mixtures. Copyright © 2013 John Wiley & Sons, Ltd.

Layer-by-layer deposition of nanostructured CsPbBr3 perovskite thin films

NASA Astrophysics Data System (ADS)

Reshetnikova, A. A.; Matyushkin, L. B.; Andronov, A. A.; Sokolov, V. S.; Aleksandrova, O. A.; Moshnikov, V. A.

2017-11-01

Layer-by-layer deposition of nanostructured perovskites cesium lead halide thin films is described. The method of deposition is based on alternate immersion of the substrate in the precursor solutions or colloidal solution of nanocrystals and methyl acetate/lead nitrate solution using the device for deposition of films by SILAR and dip-coating techniques. An example of obtaining a photosensitive structure based on nanostructures of ZnO nanowires and layers of CsBbBr3 nanocrystals is also shown.

Liquid microjunction surface sampling coupled with high-pressure liquid chromatography-electrospray ionization-mass spectrometry for analysis of drugs and metabolites in whole-body thin tissue sections.

PubMed

Kertesz, Vilmos; Van Berkel, Gary J

2010-07-15

In this work, a commercially available autosampler was adapted to perform direct liquid microjunction (LMJ) surface sampling followed by a high-pressure liquid chromatography (HPLC) separation of the extract components and detection with electrospray ionization mass spectrometry (ESI-MS). To illustrate the utility of coupling a separation with this direct liquid extraction based surface sampling approach, four different organs (brain, lung, kidney, and liver) from whole-body thin tissue sections of propranolol dosed and control mice were examined. The parent drug was observed in the chromatograms of the surface sampling extracts from all the organs of the dosed mouse examined. In addition, two isomeric phase II metabolites of propranolol (an aliphatic and an aromatic hydroxypropranolol glucuronide) were observed in the chromatograms of the extracts from lung, kidney, and liver. Confirming the presence of one or the other or both of these glucuronides in the extract from the various organs was not possible without the separation. These drug and metabolite data obtained using the LMJ surface sampling/HPLC-MS method and the results achieved by analyzing similar samples by conventional extraction of the tissues and subsequent HPLC-MS analysis were consistent. The ability to directly and efficiently sample from thin tissue sections via a liquid extraction and then perform a subsequent liquid phase separation increases the utility of this liquid extraction surface sampling approach.

Underpotential deposition-mediated layer-by-layer growth of thin films

DOEpatents

Wang, Jia Xu; Adzic, Radoslav R.

2017-06-27

A method of depositing contiguous, conformal submonolayer-to-multilayer thin films with atomic-level control is described. The process involves electrochemically exchanging a mediating element on a substrate with a noble metal film by alternatingly sweeping potential in forward and reverse directions for a predetermined number of times in an electrochemical cell. By cycling the applied voltage between the bulk deposition potential for the mediating element and the material to be deposited, repeated desorption/adsorption of the mediating element during each potential cycle can be used to precisely control film growth on a layer-by-layer basis.

Evaluation of double-layer density modulated Si thin films as Li-ion battery anodes

NASA Astrophysics Data System (ADS)

Taha Demirkan, Muhammed; Yurukcu, Mesut; Dursun, Burcu; Demir-Cakan, Rezan; Karabacak, Tansel

2017-10-01

Double-layer density modulated silicon thin films which contain alternating low and high density Si film layers were fabricated by magnetron sputtering. Two different samples consisting of alternating layers of high-density/low-density and low-density/high-density Si thin film layers were investigated as anode electrodes in Li-ion batteries. Si thin film in which the terminating layer at the top is low density Si layer-quoted as low-density/high-density film (LD/HD)- exhibits better performance than Si thin film that has high density layer at the top, -quoted as high-density/low-density (HD/LD). A highly stabilized cycling performance with the specific charge capacities of 2000 mAh g-1 at the 150th cycle at C/2 current density, and 1200 mAh g-1 at the 240th cycle at 10 C current density were observed for the LD/HD Si anode in the presence of fluoroethylene carbonate (FEC) electrolyte additive.

Evaluation of Caesalpinia bonducella flower extract for anti-inflammatory action in rats and its high performance thin layer chromatography chemical fingerprinting

PubMed Central

Arunadevi, Rathinam; Murugammal, Shanmugam; Kumar, Dinesh; Tandan, Surendra Kumar

2015-01-01

Objective: The study is aimed to evaluate anti-inflammatory activity of Caesalpinia bonducella Fleming (Caesalpiniaceae) flower extract (CBFE) and to study its effect on radiographic outcome in adjuvant induced arthritis and authentication by high performance thin layer chromatography (HPTLC) chemical fingerprinting. Materials and Methods: CBFE was administered orally (30, 100, and 300 mg/kg b.wt.) and tested for its anti-inflammatory activity in carrageenan-induced inflammation, cotton pellet induced chronic granulomatous inflammation and autacoids-induced inflammation. Effect on radiographic outcome was tested in adjuvant-induced arthritis. CBFE was HPTLC fingerprinted in suitable solvent system. Result: In carrageenan-induced inflammation, CBFE produced significant inhibition in edema volume at all the doses (30, 100 and 300 mg/kg b.wt.) and percentage of inhibition was 28.68, 31.00, and 22.48, respectively as compared to control at 5 h of its administration. In cotton pellet granuloma assay, CBFE significantly decreased the granuloma weight at 300 mg/kg dose level by 22.53%. CBFE (300 mg/kg) caused significant inhibition by 37.5, 44.44, and 35.29% edema volume, at ½, 1 and 3 h after 5-hydroxytryptamine injection, respectively. Radiographic score of animals treated with 300 mg/kg CBFE was significantly decreased when compared to arthritic control animals. Conclusion: The extract was found to possess significant anti-inflammatory activity. CBFE treatment improved the bony architecture in adjuvant-induced arthritis in rats. The developed HPTLC fingerprint would be helpful in the authentication of C. bonducella flower extract. PMID:26729956

Matching characteristics of different buffer layers with VO2 thin films

NASA Astrophysics Data System (ADS)

Yang, Kai; Zhang, Dongping; Liu, Yi; Guan, Tianrui; Qin, Xiaonan; Zhong, Aihua; Cai, Xingmin; Fan, Ping; Lv, Weizhong

2016-10-01

VO2 thin films were fabricated by reactive DC magnetron sputtering on different buffer layers of MgF2, Al2O3 and TiO2, respectively. The crystallinity and orientation relationship, thickness of VO2 thin films, atoms vibrational modes, optical and electrical property, surface morphology of films were characterized by X-ray diffraction, Raman scattering microscopy, step profiler, spectrophotometer, four-probe technique, and scanning electron microscopy, respectively. XRD results investigated that the films have preferential crystalline planes VO2 (011). The crystallinity of VO2 films grown on TiO2 buffer layers are superior to VO2 directly deposited on soda-lime glass. The Raman bands of the VO2 films correspond to an Ag symmetry mode of VO2 (M). The sample prepared on 100nm TiO2 buffer layer appears nanorods structure, and exhibits remarkable solar energy modulation ability as high as 5.82% in full spectrum and 23% in near infrared spectrum. Cross-sectional SEM image of the thin films samples indicate that MgF2 buffer layer has clear interface with VO2 layer. But there are serious interdiffusion phenomenons between Al2O3, TiO2 buffer layer with VO2 layer.

Flat-lying semiconductor-insulator interfacial layer in DNTT thin films.

PubMed

Jung, Min-Cherl; Leyden, Matthew R; Nikiforov, Gueorgui O; Lee, Michael V; Lee, Han-Koo; Shin, Tae Joo; Takimiya, Kazuo; Qi, Yabing

2015-01-28

The molecular order of organic semiconductors at the gate dielectric is the most critical factor determining carrier mobility in thin film transistors since the conducting channel forms at the dielectric interface. Despite its fundamental importance, this semiconductor-insulator interface is not well understood, primarily because it is buried within the device. We fabricated dinaphtho[2,3-b:2',3'-f]thieno[3,2-b]thiophene (DNTT) thin film transistors by thermal evaporation in vacuum onto substrates held at different temperatures and systematically correlated the extracted charge mobility to the crystal grain size and crystal orientation. As a result, we identify a molecular layer of flat-lying DNTT molecules at the semiconductor-insulator interface. It is likely that such a layer might form in other material systems as well, and could be one of the factors reducing charge transport. Controlling this interfacial flat-lying layer may raise the ultimate possible device performance for thin film devices.

System for analysis of explosives

DOEpatents

Haas, Jeffrey S [San Ramon, CA

2010-06-29

A system for analysis of explosives. Samples are spotted on a thin layer chromatography plate. Multi-component explosives standards are spotted on the thin layer chromatography plate. The thin layer chromatography plate is dipped in a solvent mixture and chromatography is allowed to proceed. The thin layer chromatography plate is dipped in reagent 1. The thin layer chromatography plate is heated. The thin layer chromatography plate is dipped in reagent 2.

Effects of different wetting layers on the growth of smooth ultra-thin silver thin films

NASA Astrophysics Data System (ADS)

Ni, Chuan; Shah, Piyush; Sarangan, Andrew M.

2014-09-01

Ultrathin silver films (thickness below 10 nm) are of great interest as optical coatings on windows and plasmonic devices. However, producing these films has been a continuing challenge because of their tendency to form clusters or islands rather than smooth contiguous thin films. In this work we have studied the effect of Cu, Ge and ZnS as wetting layers (1.0 nm) to achieve ultrasmooth thin silver films. The silver films (5 nm) were grown by RF sputter deposition on silicon and glass substrates using a few monolayers of the different wetting materials. SEM imaging was used to characterize the surface properties such as island formation and roughness. Also the optical properties were measured to identify the optical impact of the different wetting layers. Finally, a multi-layer silver based structure is designed and fabricated, and its performance is evaluated. The comparison between the samples with different wetting layers show that the designs with wetting layers which have similar optical properties to silver produce the best overall performance. In the absence of a wetting layer, the measured optical spectra show a significant departure from the model predictions, which we attribute primarily to the formation of clusters.

A tri-layer thin film containing graphene oxide to protect zinc substrates from wear

NASA Astrophysics Data System (ADS)

Wang, Ying; Gu, Zhengpeng; Yuan, Ningyi; Chu, Fuqiang; Cheng, Guanggui; Ding, Jianning

2018-06-01

Due to its excellent properties, Zn alloy is widely used in daily life. However, the poor wear-resisting properties of Zn alloys limits their application. In this paper, a tri-layer thin film consisting of 3-aminopropyltriethoxysilane (APS), graphene oxide (GO) and perfluoropolyethers (PFPE) were successfully prepared on the surface of Zn alloy to improve the wear-resisting properties. The as-prepared tri-layer thin films were characterized by atomic force microscopy, Raman spectroscopy, x-ray photoelectron spectroscopy and contact angle measurement. In addition, the tribological properties of the as-prepared tri-layer thin films were studied on a ball-on-plate tribometer and the morphologies of worn surfaces were observed using 3D noncontact interferometric microscope. Compared with the control samples, the tri-layer thin films showed excellent friction-reducing and wear-resisting properties, which was attributed to the synergistic effect of the GO as the load-carrying layer and the PFPE as the lubricating layer.

Room temperature rubbing for few-layer two-dimensional thin flakes directly on flexible polymer substrates

PubMed Central

Yu, Yan; Jiang, Shenglin; Zhou, Wenli; Miao, Xiangshui; Zeng, Yike; Zhang, Guangzu; Liu, Sisi

2013-01-01

The functional layers of few-layer two-dimensional (2-D) thin flakes on flexible polymers for stretchable applications have attracted much interest. However, most fabrication methods are “indirect” processes that require transfer steps. Moreover, previously reported “transfer-free” methods are only suitable for graphene and not for other few-layer 2-D thin flakes. Here, a friction based room temperature rubbing method is proposed for fabricating different types of few-layer 2-D thin flakes (graphene, hexagonal boron nitride (h-BN), molybdenum disulphide (MoS2), and tungsten disulphide (WS2)) on flexible polymer substrates. Commercial 2-D raw materials (graphite, h-BN, MoS2, and WS2) that contain thousands of atom layers were used. After several minutes, different types of few-layer 2-D thin flakes were fabricated directly on the flexible polymer substrates by rubbing procedures at room temperature and without any transfer step. These few-layer 2-D thin flakes strongly adhere to the flexible polymer substrates. This strong adhesion is beneficial for future applications. PMID:24045289

Bioturbation delays attenuation of DDT by clean sediment cap but promotes sequestration by thin-layered activated carbon.

PubMed

Lin, Diana; Cho, Yeo-Myoung; Werner, David; Luthy, Richard G

2014-01-21

The effects of bioturbation on the performance of attenuation by sediment deposition and activated carbon to reduce risks from DDT-contaminated sediment were assessed for DDT sediment-water flux, biouptake, and passive sampler (PE) uptake in microcosm experiments with a freshwater worm, Lumbriculus variegatus. A thin-layer of clean sediment (0.5 cm) did not reduce the DDT flux when bioturbation was present, while a thin (0.3 cm) AC cap was still capable of reducing the DDT flux by 94%. Bioturbation promoted AC sequestration by reducing the 28-day DDT biouptake (66%) and DDT uptake into PE (>99%) compared to controls. Bioturbation further promoted AC-sediment contact by mixing AC particles into underlying sediment layers, reducing PE uptake (55%) in sediment compared to the AC cap without bioturbation. To account for the observed effects from bioturbation, a mass transfer model together with a biodynamic model were developed to simulate DDT flux and biouptake, respectively, and models confirmed experimental results. Both experimental measurements and modeling predictions imply that thin-layer activated carbon placement on sediment is effective in reducing the risks from contaminated sediments in the presence of bioturbation, while natural attenuation process by clean sediment deposition may be delayed by bioturbation.

Enhanced electrical properties of dual-layer channel ZnO thin film transistors prepared by atomic layer deposition

NASA Astrophysics Data System (ADS)

Li, Huijin; Han, Dedong; Dong, Junchen; Yu, Wen; Liang, Yi; Luo, Zhen; Zhang, Shengdong; Zhang, Xing; Wang, Yi

2018-05-01

The thin film transistors (TFTs) with a dual-layer channel structure combing ZnO thin layer grown at 200 °C and ZnO film grown at 120 °C by atomic layer deposition are fabricated. The dual-layer channel TFT exhibits a low leakage current of 2.8 × 10-13 A, Ion/Ioff ratio of 3.4 × 109, saturation mobility μsat of 12 cm2 V-1 s-1, subthreshold swing (SS) of 0.25 V/decade. The SS value decreases to 0.18 V/decade after the annealing treatment in O2 due to the reduction of the trap states at the channel/dielectric interface and in the bulk channel layer. The enhanced performance obtained from the dual-layer channel TFTs is due to the ability of maintaining high mobility and suppressing the increase in the off-current at the same time.

Liquid Chromatography-Mass Spectrometry-based Quantitative Proteomics

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

Xie, Fang; Liu, Tao; Qian, Weijun

2011-07-22

Liquid chromatography-mass spectrometry (LC-MS)-based quantitative proteomics has become increasingly applied for a broad range of biological applications due to growing capabilities for broad proteome coverage and good accuracy in quantification. Herein, we review the current LC-MS-based quantification methods with respect to their advantages and limitations, and highlight their potential applications.

Process for forming epitaxial perovskite thin film layers using halide precursors

DOEpatents

Clem, Paul G.; Rodriguez, Mark A.; Voigt, James A.; Ashley, Carol S.

2001-01-01

A process for forming an epitaxial perovskite-phase thin film on a substrate. This thin film can act as a buffer layer between a Ni substrate and a YBa.sub.2 Cu.sub.3 O.sub.7-x superconductor layer. The process utilizes alkali or alkaline metal acetates dissolved in halogenated organic acid along with titanium isopropoxide to dip or spin-coat the substrate which is then heated to about 700.degree. C. in an inert gas atmosphere to form the epitaxial film on the substrate. The YBCO superconductor can then be deposited on the layer formed by this invention.

Density-controlled, solution-based growth of ZnO nanorod arrays via layer-by-layer polymer thin films for enhanced field emission

NASA Astrophysics Data System (ADS)

Weintraub, Benjamin; Chang, Sehoon; Singamaneni, Srikanth; Han, Won Hee; Choi, Young Jin; Bae, Joonho; Kirkham, Melanie; Tsukruk, Vladimir V.; Deng, Yulin

2008-10-01

A simple, scalable, and cost-effective technique for controlling the growth density of ZnO nanorod arrays based on a layer-by-layer polyelectrolyte polymer film is demonstrated. The ZnO nanorods were synthesized using a low temperature (T = 90 °C), solution-based method. The density-control technique utilizes a polymer thin film pre-coated on the substrate to control the mass transport of the reactant to the substrate. The density-controlled arrays were investigated as potential field emission candidates. The field emission results revealed that an emitter density of 7 nanorods µm-2 and a tapered nanorod morphology generated a high field enhancement factor of 5884. This novel technique shows promise for applications in flat panel display technology.

Synthesis and Characterization of Hydrophobic Silica Thin Layer Derived from Methyltrimethoxysilane (MTMS)

NASA Astrophysics Data System (ADS)

Darmawan, Adi; Utari, Riyadini; Eka Saputra, Riza; Suhartana; Astuti, Yayuk

2018-01-01

This study investigated the synthesis and characterization of MTMS hydrophobic silica prepared by sol-gel method. In principle, silica xerogels and silica thin layer were obtained by reacting MTMS in ethanol solvent in some pH variations. The MTMS solution was used to modify the surface of the ceramic plate by dipcoating method to further be calcined at two different temperatures of 350°C and 500°C. The silica xerogels were analysed by FTIR, TGA-DSC and GSA to determine functional group characteristics, thermal properties and pore morphology respectively. Meanwhile, the silica thin layers were analysed their hydrophobic properties using water contact angle measurement and surface roughness determination using SEM. The results showed that the higher the pH used in the MTMS solution, the higher the resulting contact angle. The highest contact angle was obtained at pH 8.12 which reached 94.7° and 79.5° for silica thin layer calcined at 350°C and 500°C, respectively. The TGA results indicated that the methyl group survived up to 400°C and disappeared at 500°C which had implications on silica thin layer hydrophobic nature. GSA result exhibited that the silica xerogel had a close structure with a very low pore volume. While the SEM-EDX results displayed that the silica thin layer prepared at acidic pH had smoother surface morphology and became rough when prepared at an alkaline pH.

Simultaneous determination of atenolol and amlodipine in tablets by high-performance thin-layer chromatography.

PubMed

Argekar, A P; Powar, S G

2000-01-01

A new simple, precise, rapid and selective high-performance thin-layer chromatographic (HPTLC) method has been developed for the simultaneous determination of atenolol (ATL) and amlodipine (AMLO) in tablets, using methylene chloride:methanol:ammonia solution (25% NH3) (8.8:1.3:0.1; v/v) as the mobile phase and Merck HPTLC plates (0.2 mm thickness) precoated with 60F254 silica gel on aluminium sheet as the stationary phase. Detection was carried out densitometrically using a UV detector at 230 nm. The retention factors of ATL and AMLO were 0.33 and 0.75, respectively. Calibration curves were linear in the range 10-500 microg ml(-1) for both. Assays of ATL and AMLO were 49.87 mg per tablet (relative standard deviation (R.S.D.), 1.3%) and 4.90 mg per tablet (R.S.D., 1.38%) for brand I, and 49.27 mg per tablet (R.S.D., 1.12%) and 4.98 mg per tablet (R.S.D., 1.42%) for brand II, respectively. The percentage recoveries for ATL and AMLO for brands I and II were 99.06 and 99.30%, and 99.27 and 99.15%, respectively.

Validated stability-indicating densitometric thin-layer chromatography: application to stress degradation studies of minocycline.

PubMed

Jain, Nilu; Jain, Gaurav Kumar; Ahmad, Farhan Jalees; Khar, Roop Krishen

2007-09-19

A simple, stability-indicating high-performance thin-layer liquid chromatographic (HPTLC) method for analysis of minocycline was developed and validated. The densitometric analysis was carried out at 345 nm using methanol-acetonitrile-isopropyl alcohol-water (5:4:0.5:0.5, v/v/v/v) as mobile phase. The method employed TLC aluminium plates pre-coated with silica gel 60F-254 as the stationary phase. To achieve good result, plates were sprayed with a 10% (w/v) solution of disodium ethylene diaminetetraacetic acid (EDTA), the pH of which was adjusted to 9.0. Compact spots of minocycline were found at R(f) = 0.30+/-0.02. For proposed procedure, linearity (r = 0.9997), limit of detection (3.7 ng spot(-1)), recovery (99.23-100.16%), and precision (% R.S.D. < or = 0.364) was found to be satisfactory. The drug undergoes acidic and basic degradation, oxidation and photodegradation. All the peaks of degradation products were well resolved from the pure drug with significantly different R(f) values. The acidic and alkaline degradation kinetics of minocycline, evaluated using this method, is found to be of first order.

The Use of Gas Chromatography and Mass Spectrometry to Introduce General Chemistry Students to Percent Mass and Atomic Mass Calculations

ERIC Educational Resources Information Center

Pfennig, Brian W.; Schaefer, Amy K.

2011-01-01

A general chemistry laboratory experiment is described that introduces students to instrumental analysis using gas chromatography-mass spectrometry (GC-MS), while simultaneously reinforcing the concepts of mass percent and the calculation of atomic mass. Working in small groups, students use the GC to separate and quantify the percent composition…

Nucleation and growth kinetics during metal-induced layer exchange crystallization of Ge thin films at low temperatures

NASA Astrophysics Data System (ADS)

Hu, Shu; McIntyre, Paul C.

2012-02-01

The kinetics of Al-catalyzed layer exchange crystallization of amorphous germanium (Ge) thin films at low temperatures is reported. Observation of Ge mass transport from an underlying amorphous Ge layer to the Al film surface through an interposed sub-nanometer GeOx interfacial layer allows independent measurement of the areal density and average area of crystalline Ge islands formed on the film surface. We show that bias-voltage stressing of the interfacial layer can be used to control the areal density of nucleated Ge islands. Based on experimental observations, the Johnson-Mehl-Avrami-Kolmogorov phase transformation theory is used to model nanoscale nucleation and growth of Ge islands in two dimensions. Ge island nucleation kinetics follows an exponentially decaying nucleation rate with time. Ge island growth kinetics switches from linear growth at a constant growth velocity to diffusion-limited growth as the growth front advances. The transition point between these two regimes depends on the Ge nucleation site density and the annealing temperature. Knowledge of the kinetics of low-temperature crystallization is important in achieving textured polycrystalline Ge thin films with large grains for applications in large-area electronics and solar energy conversion.

Fabrication of Crack-Free Barium Titanate Thin Film with High Dielectric Constant Using Sub-Micrometric Scale Layer-by-Layer E-Jet Deposition.

PubMed

Liang, Junsheng; Li, Pengfei; Wang, Dazhi; Fang, Xu; Ding, Jiahong; Wu, Junxiong; Tang, Chang

2016-01-19

Dense and crack-free barium titanate (BaTiO₃, BTO) thin films with a thickness of less than 4 μm were prepared by using sub-micrometric scale, layer-by-layer electrohydrodynamic jet (E-jet) deposition of the suspension ink which is composed of BTO nanopowder and BTO sol. Impacts of the jet height and line-to-line pitch of the deposition on the micro-structure of BTO thin films were investigated. Results show that crack-free BTO thin films can be prepared with 4 mm jet height and 300 μm line-to-line pitch in this work. Dielectric constant of the prepared BTO thin film was recorded as high as 2940 at 1 kHz at room temperature. Meanwhile, low dissipation factor of the BTO thin film of about 8.6% at 1 kHz was also obtained. The layer-by-layer E-jet deposition technique developed in this work has been proved to be a cost-effective, flexible and easy to control approach for the preparation of high-quality solid thin film.

Fabrication of Crack-Free Barium Titanate Thin Film with High Dielectric Constant Using Sub-Micrometric Scale Layer-by-Layer E-Jet Deposition

PubMed Central

Liang, Junsheng; Li, Pengfei; Wang, Dazhi; Fang, Xu; Ding, Jiahong; Wu, Junxiong; Tang, Chang

2016-01-01

Dense and crack-free barium titanate (BaTiO3, BTO) thin films with a thickness of less than 4 μm were prepared by using sub-micrometric scale, layer-by-layer electrohydrodynamic jet (E-jet) deposition of the suspension ink which is composed of BTO nanopowder and BTO sol. Impacts of the jet height and line-to-line pitch of the deposition on the micro-structure of BTO thin films were investigated. Results show that crack-free BTO thin films can be prepared with 4 mm jet height and 300 μm line-to-line pitch in this work. Dielectric constant of the prepared BTO thin film was recorded as high as 2940 at 1 kHz at room temperature. Meanwhile, low dissipation factor of the BTO thin film of about 8.6% at 1 kHz was also obtained. The layer-by-layer E-jet deposition technique developed in this work has been proved to be a cost-effective, flexible and easy to control approach for the preparation of high-quality solid thin film. PMID:28787860

Normal Raman and surface enhanced Raman spectroscopic experiments with thin layer chromatography spots of essential amino acids using different laser excitation sources.

PubMed

István, Krisztina; Keresztury, Gábor; Szép, Andrea

2003-06-01

A comparative study of the feasibility and efficiency of Raman spectroscopic detection of thin layer chromatography (TLC) spots of some weak Raman scatterers (essential amino acids, namely, glycine and L-forms of alanine, serine, valine, proline, hydroxyproline, and phenylalanine) was carried out using four different visible and near-infrared (NIR) laser radiations with wavelengths of 532, 633, 785, and 1064 nm. Three types of commercial TLC plates were tested and the possibility of inducing surface enhanced Raman scattering (SERS) by means of Ag-sol was also investigated. The spectra obtained from spotted analytes adsorbed on TLC plates were of very different quality strongly depending on the excitation wavelength, the wetness of the samples, and the compounds examined. The best results were obtained with the simple silica TLC plate, and it has been established that the longest wavelength (lowest energy) NIR excitation of a Nd:YAG laser is definitely more suitable for generating normal Raman scattering of analyte spots than any of the visible radiations. Concerning SERS with application of Ag-sol to the TLC spots, 1-3 orders of magnitude enhancement was observed with wet samples, the greatest with the 532 nm radiation and gradually smaller with the longer wavelength excitations. It is shown, however, that due to severe adsorption-induced spectral distortions and increased sensitivity to microscopic inhomogeneity of the sample, none of the SERS spectra obtained with the dispersive Raman microscope operating in the visible region were superior to the best NIR normal FT-Raman spectra, as far as sample identification is concerned.

Normal Raman and surface enhanced Raman spectroscopic experiments with thin layer chromatography spots of essential amino acids using different laser excitation sources

NASA Astrophysics Data System (ADS)

István, Krisztina; Keresztury, Gábor; Szép, Andrea

2003-06-01

A comparative study of the feasibility and efficiency of Raman spectroscopic detection of thin layer chromatography (TLC) spots of some weak Raman scatterers (essential amino acids, namely, glycine and L-forms of alanine, serine, valine, proline, hydroxyproline, and phenylalanine) was carried out using four different visible and near-infrared (NIR) laser radiations with wavelengths of 532, 633, 785, and 1064 nm. Three types of commercial TLC plates were tested and the possibility of inducing surface enhanced Raman scattering (SERS) by means of Ag-sol was also investigated. The spectra obtained from spotted analytes adsorbed on TLC plates were of very different quality strongly depending on the excitation wavelength, the wetness of the samples, and the compounds examined. The best results were obtained with the simple silica TLC plate, and it has been established that the longest wavelength (lowest energy) NIR excitation of a Nd:YAG laser is definitely more suitable for generating normal Raman scattering of analyte spots than any of the visible radiations. Concerning SERS with application of Ag-sol to the TLC spots, 1-3 orders of magnitude enhancement was observed with wet samples, the greatest with the 532 nm radiation and gradually smaller with the longer wavelength excitations. It is shown, however, that due to severe adsorption-induced spectral distortions and increased sensitivity to microscopic inhomogeneity of the sample, none of the SERS spectra obtained with the dispersive Raman microscope operating in the visible region were superior to the best NIR normal FT-Raman spectra, as far as sample identification is concerned.

Investigation of the superconducting proximity effect (SPE) and magnetic dead layers (MDL) in thin film double layers

NASA Astrophysics Data System (ADS)

Tateishi, Go

When a thin superconducting film (S film) is condensed onto a thin normal conducting film (N film), the first layers of the S film loose their superconductivity. This phenomenon is generally called the "superconducting proximity effect (SPE)". As an investigation of SPE we focus on the transition temperature of extremely thin NS double layers in the thin regime. Normal metal is condensed on top of insulating Sb, then Pb is deposited on it in small steps. The transition temperature is plotted in an inverse Tc-reduction 1/Delta T c =1/(Ts - Tc) versus Pb thickness graph. To compare our experimental results with the theoretical prediction, a numerical calculation of the SN double layer is performed by our group using the linear gap equation. As a result, there are large discrepancies between the experimental and theoretical results generally. The results of the NS double layers can be divided into three groups in terms of their discrepancies between experiment and theory.(1) Non-coupling (Tc = 0 K): N= Mg, Ag, Cu, Au. There are large deviations between experiment and theory by a factor to the order of 2.5. (2) Weak coupling (Tc is low (< 2.5 K)) : N=Cd, Zn, Al. Deviation is present, but only by a factor of 1.5. (3) Intermediate coupling (T c is around half of Pb's (≈ 4.5 K)) : N=In, Sn. The experimental results agree with the theory. Next, we examine the detection of the magnetic dead layer (MDL) of Ni thin films in terms of the anomalous Hall effect (AHE) with several non-magnetic metal substrates. In our results, when Ni film is contact with a polyvalent metal substrate film, the sandwich film has around 2 to 3.5 at.lay. of magnetic dead layers. However we have not observed the magnetic dead Ni layers with the alkali and noble metal substrate film. Finally, we revisit the Pb/Ni system to measure the magnetic scattering of Ni with the method of Weak Localization (WL) to compare with the dephasing rate due to the Tc-reduction. In this series, we use only very thin

Spectral, thermal and optical-electrical properties of the layer-by-layer deposited thin film of nano Zn(II)-8-hydroxy-5-nitrosoquinolate complex.

PubMed

Haggag, Sawsan M S; Farag, A A M; Abdelrafea, Mohamed

2013-06-01

Zinc(II)-8-hydroxy-5-nitrosoquinolate, [Zn(II)-(HNOQ)2], was synthesized and assembled as a deposited thin film of nano-metal complex by a rapid, direct, simple and efficient procedure based on layer-by-layer chemical deposition technique. Stoichiometric identification and structural characterization of [Zn(II)-(HNOQ)2] were confirmed by electron impact mass spectrometry (EI-MS) and Fourier Transform infrared spectroscopy (FT-IR). Surface morphology was studied by using a scanning electron microscope imaging (SEM) and the particle size was found to be in the range of 23-49 nm. Thermal stability of [Zn(II)-(HNOQ)2] was studied and the thermal parameters were evaluated using thermal gravimetric analysis (TGA). The current density-voltage measurements showed that the current flow is dominated by a space charge limited and influenced by traps under high bias. The optical properties of [Zn(II)-(HNOQ)2] thin films were found to exhibit two direct allowed transitions at 2.4 and 1.0 eV, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

Selective Nanoscale Mass Transport across Atomically Thin Single Crystalline Graphene Membranes.

PubMed

Kidambi, Piran R; Boutilier, Michael S H; Wang, Luda; Jang, Doojoon; Kim, Jeehwan; Karnik, Rohit

2017-05-01

Atomically thin single crystals, without grain boundaries and associated defect clusters, represent ideal systems to study and understand intrinsic defects in materials, but probing them collectively over large area remains nontrivial. In this study, the authors probe nanoscale mass transport across large-area (≈0.2 cm 2 ) single-crystalline graphene membranes. A novel, polymer-free picture frame assisted technique, coupled with a stress-inducing nickel layer is used to transfer single crystalline graphene grown on silicon carbide substrates to flexible polycarbonate track etched supports with well-defined cylindrical ≈200 nm pores. Diffusion-driven flow shows selective transport of ≈0.66 nm hydrated K + and Cl - ions over ≈1 nm sized small molecules, indicating the presence of selective sub-nanometer to nanometer sized defects. This work presents a framework to test the barrier properties and intrinsic quality of atomically thin materials at the sub-nanometer to nanometer scale over technologically relevant large areas, and suggests the potential use of intrinsic defects in atomically thin materials for molecular separations or desalting. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Thin layer drying of cassava starch using continuous vibrated fluidized bed dryer

NASA Astrophysics Data System (ADS)

Suherman, Trisnaningtyas, Rona

2015-12-01

This paper present the experimental work and thin layer modelling of cassava starch drying in continuous vibrated fluidized bed dryer. The experimental data was used to validate nine thin layer models of drying curve. Cassava starch with 0.21 initial moisture content was dried in different air drying temperature (50°C, 55°C, 60°C, 65°C, 70°C), different weir height in bed (0 and 1 cm), and different solid feed flow (10 and 30 gr.minute-1). The result showed air dryer temperature has a significant effect on drying curve, while the weir height and solid flow rate are slightly. Based on value of R2, χ2, and RMSE, Page Model is the most accurate simulation for thin layer drying model of cassava starch.

Screening anti-tumor compounds from Ligusticum wallichii using cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry.

PubMed

Zhang, Tao; Ding, Yuanyuan; An, Hongli; Feng, Liuxin; Wang, Sicen

2015-07-14

Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry was developed. Tyrosine 367 Cysteine-HEK293 cells were used as cell membrane stationary phase. Specificity and reproducibility of the cell membrane chromatography was evaluated using 1-tert-butyl-3-{2-[4-(diethylamino)butylamino]-6-(3,5-dimethoxyphenyl)pyrido[2,3-d]pyrimidin-7-yl}urea, Nimodipine and dexamethasone acetate. Then, anti-tumor components acting on Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 were screened and identified from extracts of Ligusticum wallichii. Components from the extract were retained on the cell membrane chromatographic column. The retained fraction was directly eluted into high-performance liquid chromatography with mass spectrometry system for separation and identification. Finally, Levistolide A was identified as an active component from Ligusticum wallichii extracts. The 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-tetrazolium bromide-formazan colorimetric assay revealed that Levistolide A inhibits proliferation of overexpressing the mutated receptor cells with dose-dependent manner. Phosphorylation of fibroblast growth factor receptor 4 was also decrease under Levistolide A treatment. Flex dock simulation verified that Levistolide A could bind with the tyrosine kinase domain of fibroblast growth factor receptor 4. Therefore, Levistolide A screened by the cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry can arrest cell growth. In conclusion, the two-dimensional high-performance liquid chromatography method can screen and identify potential anti-tumor ingredients which specifically act on the tyrosine kinase domain of the mutated fibroblast growth factor receptor 4. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

Effect of dual-dielectric hydrogen-diffusion barrier layers on the performance of low-temperature processed transparent InGaZnO thin-film transistors

NASA Astrophysics Data System (ADS)

Tari, Alireza; Wong, William S.

2018-02-01

Dual-dielectric SiOx/SiNx thin-film layers were used as back-channel and gate-dielectric barrier layers for bottom-gate InGaZnO (IGZO) thin-film transistors (TFTs). The concentration profiles of hydrogen, indium, gallium, and zinc oxide were analyzed using secondary-ion mass spectroscopy characterization. By implementing an effective H-diffusion barrier, the hydrogen concentration and the creation of H-induced oxygen deficiency (H-Vo complex) defects during the processing of passivated flexible IGZO TFTs were minimized. A bilayer back-channel passivation layer, consisting of electron-beam deposited SiOx on plasma-enhanced chemical vapor-deposition (PECVD) SiNx films, effectively protected the TFT active region from plasma damage and minimized changes in the chemical composition of the semiconductor layer. A dual-dielectric PECVD SiOx/PECVD SiNx gate-dielectric, using SiOx as a barrier layer, also effectively prevented out-diffusion of hydrogen atoms from the PECVD SiNx-gate dielectric to the IGZO channel layer during the device fabrication.

Polymer Analysis by Liquid Chromatography/Electrospray Ionization Time-of-Flight Mass Spectrometry.

PubMed

Nielen, M W; Buijtenhuijs, F A

1999-05-01

Hyphenation of liquid chromatography (LC) techniques with electrospray ionization (ESI) orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS) provides both MS-based structural information and LC-based quantitative data in polymer analysis. In one experimental setup, three different LC modes are interfaced with MS:  size-exclusion chromatography (SEC/MS), gradient polymer elution chromatography (GPEC/MS), and liquid chromatography at the critical point of adsorption (LCCC/MS). In SEC/MS, both absolute mass calibration of the SEC column based on the polymer itself and determination of monomers and end groups from the mass spectra are achieved. GPEC/MS shows detailed chemical heterogeneity of the polymer and the chemical composition distribution within oligomer groups. In LCCC/MS, the retention behavior is primarily governed by chemical heterogeneities, such as different end group functionalities, and quantitative end group calculations can be easily made. The potential of these methods and the benefit of time-of-flight analyzers in polymer analysis are discussed using SEC/MS of a polydisperse poly(methyl methacrylate) sample, GPEC/MS of dipropoxylated bisphenol A/adipic acid polyester resin, LCCC/MS of alkylated poly(ethylene glycol), and LCCC/MS of terephthalic acid/neopentyl glycol polyester resin.

Underpotential deposition-mediated layer-by-layer growth of thin films

DOEpatents

Wang, Jia Xu; Adzic, Radoslav R.

2015-05-19

A method of depositing contiguous, conformal submonolayer-to-multilayer thin films with atomic-level control is described. The process involves the use of underpotential deposition of a first element to mediate the growth of a second material by overpotential deposition. Deposition occurs between a potential positive to the bulk deposition potential for the mediating element where a full monolayer of mediating element forms, and a potential which is less than, or only slightly greater than, the bulk deposition potential of the material to be deposited. By cycling the applied voltage between the bulk deposition potential for the mediating element and the material to be deposited, repeated desorption/adsorption of the mediating element during each potential cycle can be used to precisely control film growth on a layer-by-layer basis. This process is especially suitable for the formation of a catalytically active layer on core-shell particles for use in energy conversion devices such as fuel cells.

Analysis of small carbohydrates in several bioactive botanicals by gas chromatography with mass spectrometry and liquid chromatography with tandem mass spectrometry.

PubMed

Moldoveanu, Serban; Scott, Wayne; Zhu, Jeff

2015-11-01

Bioactive botanicals contain natural compounds with specific biological activity, such as antibacterial, antioxidant, immune stimulating, and taste improving. A full characterization of the chemical composition of these botanicals is frequently necessary. A study of small carbohydrates from the plant materials of 18 bioactive botanicals is further described. The study presents the identification of the carbohydrate using a gas chromatographic-mass spectrometric analysis that allows detection of molecules as large as maltotetraose, after changing them into trimethylsilyl derivatives. A number of carbohydrates in the plant (fructose, glucose, mannose, sucrose, maltose, xylose, sorbitol, and myo-, chiro-, and scyllo-inositols) were quantitated using a novel liquid chromatography with tandem mass spectrometric technique. Both techniques involved new method developments. The gas chromatography with mass spectrometric analysis involved derivatization and separation on a Rxi(®)-5Sil MS column with H2 as a carrier gas. The liquid chromatographic separation was obtained using a hydrophilic interaction type column, YMC-PAC Polyamine II. The tandem mass spectrometer used an electrospray ionization source in multiple reaction monitoring positive ion mode with the detection of the adducts of the carbohydrates with Cs(+) ions. The validated quantitative procedure showed excellent precision and accuracy allowing the analysis in a wide range of concentrations of the analytes. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Deposition of ultra thin CuInS₂ absorber layers by ALD for thin film solar cells at low temperature (down to 150 °C).

PubMed

Schneider, Nathanaelle; Bouttemy, Muriel; Genevée, Pascal; Lincot, Daniel; Donsanti, Frédérique

2015-02-06

Two new processes for the atomic layer deposition of copper indium sulfide (CuInS₂) based on the use of two different sets of precursors are reported. Metal chloride precursors (CuCl, InCl₃) in combination with H2S imply relatively high deposition temperature (Tdep = 380 °C), and due to exchange reactions, CuInS₂ stoechiometry was only achieved by depositing In₂S3 layers on a CuxS film. However, the use of acac- metal precursors (Cu(acac)₂, In(acac)₃) allows the direct deposition of CuInS₂ at temperature as low as 150 °C, involving in situ copper-reduction, exchange reaction and diffusion processes. The morphology, crystallographic structure, chemical composition and optical band gap of thin films were investigated using scanning electronic microscope, x-ray diffraction under grazing incidence conditions, x-ray fluorescence, energy dispersive spectrometry, secondary ion mass spectrometry, x-ray photoelectron spectroscopy and UV-vis spectroscopy. Films were implemented as ultra-thin absorbers in a typical CIS-solar cell architecture and allowed conversion efficiencies up to 2.8%.

Co-precipitation of tobramycin into biomimetically coated orthopedic fixation pins employing submicron-thin seed layers of hydroxyapatite.

PubMed

Sörensen, Jan H; Lilja, Mirjam; Åstrand, Maria; Sörensen, Torben C; Procter, Philip; Strømme, Maria; Steckel, Hartwig

2014-01-01

The migration, loosening and cut-out of implants and nosocomial infections are current problems associated with implant surgery. New innovative strategies to overcome these issues are emphasized in today's research. The current work presents a novel strategy involving co-precipitation of tobramycin with biomimetic hydroxyapatite (HA) formation to produce implant coatings that control local drug delivery to prevent early bacterial colonization of the implant. A submicron- thin HA layer served as seed layer for the co-precipitation process and allowed for incorporation of tobramycin in the coating from a stock solution of antibiotic concentrations as high as 20 mg/ml. Concentrations from 0.5 to 20 mg/ml tobramycin and process temperatures of 37 °C and 60 °C were tested to assess the optimal parameters for a thin tobramycin- delivering HA coating on discs and orthopedic fixation pins. The morphology and thickness of the coating and the drug-release profile were evaluated via scanning electron microscopy and high performance liquid chromatography. The coatings delivered pharmaceutically relevant amounts of tobramycin over a period of 12 days. To the best of our knowledge, this is the longest release period ever observed for a fast-loaded biomimetic implant coating. The presented approach could form the foundation for development of combination device/antibiotic delivery vehicles tailored to meet well-defined clinical needs while combating infections and ensuring fast implant in-growth.

Disruption of vertical motility by shear triggers formation of thin phytoplankton layers.

PubMed

Durham, William M; Kessler, John O; Stocker, Roman

2009-02-20

Thin layers of phytoplankton are important hotspots of ecological activity that are found in the coastal ocean, meters beneath the surface, and contain cell concentrations up to two orders of magnitude above ambient concentrations. Current interpretations of their formation favor abiotic processes, yet many phytoplankton species found in these layers are motile. We demonstrated that layers formed when the vertical migration of phytoplankton was disrupted by hydrodynamic shear. This mechanism, which we call gyrotactic trapping, can be responsible for the thin layers of phytoplankton commonly observed in the ocean. These results reveal that the coupling between active microorganism motility and ambient fluid motion can shape the macroscopic features of the marine ecological landscape.

Application of thin-layer Navier-Stokes equations near maximum lift

NASA Technical Reports Server (NTRS)

Anderson, W. K.; Thomas, J. L.; Rumsey, C. L.

1984-01-01

The flowfield about a NACA 0012 airfoil at a Mach number of 0.3 and Reynolds number of 1 million is computed through an angle of attack range, up to 18 deg, corresponding to conditions up to and beyond the maximum lift coefficient. Results obtained using the compressible thin-layer Navier-Stokes equations are presented as well as results from the compressible Euler equations with and without a viscous coupling procedure. The applicability of each code is assessed and many thin-layer Navier-Stokes benchmark solutions are obtained which can be used for comparison with other codes intended for use at high angles of attack. Reasonable agreement of the Navier-Stokes code with experiment and the viscous-inviscid interaction code is obtained at moderate angles of attack. An unsteady solution is obtained with the thin-layer Navier-Stokes code at the highest angle of attack considered. The maximum lift coefficient is overpredicted, however, in comparison to experimental data, which is attributed to the presence of a laminar separation bubble near the leading edge not modeled in the computations. Two comparisons with experimental data are also presented at a higher Mach number.

Breakthrough to Non-Vacuum Deposition of Single-Crystal, Ultra-Thin, Homogeneous Nanoparticle Layers: A Better Alternative to Chemical Bath Deposition and Atomic Layer Deposition

PubMed Central

Liao, Yu-Kuang; Liu, Yung-Tsung; Hsieh, Dan-Hua; Shen, Tien-Lin; Hsieh, Ming-Yang; Tzou, An-Jye; Chen, Shih-Chen; Tsai, Yu-Lin; Lin, Wei-Sheng; Chan, Sheng-Wen; Shen, Yen-Ping; Cheng, Shun-Jen; Chen, Chyong-Hua; Wu, Kaung-Hsiung; Chen, Hao-Ming; Kuo, Shou-Yi; Charlton, Martin D. B.; Hsieh, Tung-Po; Kuo, Hao-Chung

2017-01-01

Most thin-film techniques require a multiple vacuum process, and cannot produce high-coverage continuous thin films with the thickness of a few nanometers on rough surfaces. We present a new ”paradigm shift” non-vacuum process to deposit high-quality, ultra-thin, single-crystal layers of coalesced sulfide nanoparticles (NPs) with controllable thickness down to a few nanometers, based on thermal decomposition. This provides high-coverage, homogeneous thickness, and large-area deposition over a rough surface, with little material loss or liquid chemical waste, and deposition rates of 10 nm/min. This technique can potentially replace conventional thin-film deposition methods, such as atomic layer deposition (ALD) and chemical bath deposition (CBD) as used by the Cu(In,Ga)Se2 (CIGS) thin-film solar cell industry for decades. We demonstrate 32% improvement of CIGS thin-film solar cell efficiency in comparison to reference devices prepared by conventional CBD deposition method by depositing the ZnS NPs buffer layer using the new process. The new ZnS NPs layer allows reduction of an intrinsic ZnO layer, which can lead to severe shunt leakage in case of a CBD buffer layer. This leads to a 65% relative efficiency increase. PMID:28383488

Atomically thin transition metal layers: Atomic layer stabilization and metal-semiconductor transition

NASA Astrophysics Data System (ADS)

Hwang, Jeongwoon; Oh, Young Jun; Kim, Jiyoung; Sung, Myung Mo; Cho, Kyeongjae

2018-04-01

We have performed first-principle calculations to explore the possibility of synthesizing atomically thin transition metal (TM) layers. Buckled structures as well as planar structures of elemental 2D TM layers result in significantly higher formation energies compared with sp-bonded elemental 2D materials with similar structures, such as silicene and phosphorene. It is shown that the TM layers can be stabilized by surface passivation with HS, C6H5S2, or O, and O passivation is most effective. The surface oxygen passivation can improve stability leading to thermodynamically stable TM monolayers except Au, which is the most non-reactive metal element. Such stabilized TM monolayers also show an electronic structure transition from metallic state of free-standing TM layer to semiconducting O-passivated Mo and W monolayers with band gaps of 0.20-1.38 eV.

Highway pavement performance test for colored thin anti-skidding layers

NASA Astrophysics Data System (ADS)

Gao, Wei; Cui, Wei; Xu, Ming

2018-03-01

Based on the actual service condition of highway pavement colored thin anti-skidding layers, with materials of color quartz sand and two-component acrylic resin as basis, we designed such tests as the bond strength, shearing strength, tear strength, fatigue performance and aggregate polished value, and included the freeze-thaw cycle and de-icing salt and other factors in the experiment, connecting with the climate characteristics of circumpolar latitude and low altitude in Heilongjiang province. Through the pavement performance test, it is confirmed that the colored thin anti-skidding layers can adapt to cold and humid climate conditions, and its physical mechanical properties are good.

Optical Properties of Hybrid Inorganic/Organic Thin Film Encapsulation Layers for Flexible Top-Emission Organic Light-Emitting Diodes.

PubMed

An, Jae Seok; Jang, Ha Jun; Park, Cheol Young; Youn, Hongseok; Lee, Jong Ho; Heo, Gi-Seok; Choi, Bum Ho; Lee, Choong Hun

2015-10-01

Inorganic/organic hybrid thin film encapsulation layers consist of a thin Al2O3 layer together with polymer material. We have investigated optical properties of thin film encapsulation layers for top-emission flexible organic light-emitting diodes. The transmittance of hybrid thin film encapsulation layers and the electroluminescent spectrum of organic light-emitting diodes that were passivated by hybrid organic/inorganic thin film encapsulation layers were also examined as a function of the thickness of inorganic Al203 and monomer layers. The number of interference peaks, their intensity, and their positions in the visible range can be controlled by varying the thickness of inorganic Al2O3 layer. On the other hand, changing the thickness of monomer layer had a negligible effect on the optical properties. We also verified that there is a trade-off between transparency in the visible range and the permeation of water vapor in hybrid thin film encapsulation layers. As the number of dyads decreased, optical transparency improved while the water vapor permeation barrier was degraded. Our study suggests that, in top-emission organic light-emitting diodes, the thickness of each thin film encapsulation layer, in particular that of the inorganic layer, and the number of dyads should be controlled for highly efficient top-emission flexible organic light-emitting diodes.

Ultrasonic measurements of thin zinc layers on concrete

NASA Astrophysics Data System (ADS)

Jansen, Henri; Brooks, Bill; Nguyen, Vinh; Koretsky, Milo

2008-05-01

In order to protect bridges at the coast from corrosion, a thin layer (approximately 0.5 mm) of zinc is sprayed on the concrete of the bridge. When this zinc layer is electrically connected to the reinforcing steel (rebar) and placed at a positive potential with respect to the rebar, oxidation is favored at the zinc layer and reduced at the rebar. The resulting protection of the rebar fails when the zinc layer delaminates from the concrete or when the zinc oxidation product layer becomes too thick. We have used ultrasonic detection to investigate the properties of the zinc layer. This method has been applied very successfully in the semiconductor industry. We present the details of the method and the expected response. Unfortunately, we are not able to measure changes in the zinc layer, because either the frequency we use (10-20 MHz) is too low, or scattering in the concrete is a dominant effect.

Characterization of Softmagnetic Thin Layers Using Barkhausen Noise Microscopy

DTIC Science & Technology

2001-04-01

magnetoresistive (MR) sensors softmagnetic thin layer systems are used. Optimal performance of these layers requires homogeneous magnetic properties , especially a...Sendust, used in inductive sensors and nanocrystalline NiFe , used in MR-sensors. In quality correlations to Barkhausen noise parameters were found...Brillouin scattering are frequently used. An important issue is the influence of mechanical properties , e.g. residual stress on the magnetic performance

Thin film solar cell including a spatially modulated intrinsic layer

DOEpatents

Guha, Subhendu; Yang, Chi-Chung; Ovshinsky, Stanford R.

1989-03-28

One or more thin film solar cells in which the intrinsic layer of substantially amorphous semiconductor alloy material thereof includes at least a first band gap portion and a narrower band gap portion. The band gap of the intrinsic layer is spatially graded through a portion of the bulk thickness, said graded portion including a region removed from the intrinsic layer-dopant layer interfaces. The band gap of the intrinsic layer is always less than the band gap of the doped layers. The gradation of the intrinsic layer is effected such that the open circuit voltage and/or the fill factor of the one or plural solar cell structure is enhanced.

Analysis of layer-by-layer thin-film oxide growth using RHEED and Atomic Force Microscopy

NASA Astrophysics Data System (ADS)

Adler, Eli; Sullivan, M. C.; Gutierrez-Llorente, Araceli; Joress, H.; Woll, A.; Brock, J. D.

2015-03-01

Reflection high energy electron diffraction (RHEED) is commonly used as an in situ analysis tool for layer-by-layer thin-film growth. Atomic force microscopy is an equally common ex situ tool for analysis of the film surface, providing visual evidence of the surface morphology. During growth, the RHEED intensity oscillates as the film surface changes in roughness. It is often assumed that the maxima of the RHEED oscillations signify a complete layer, however, the oscillations in oxide systems can be misleading. Thus, using only the RHEED maxima is insufficient. X-ray reflectivity can also be used to analyze growth, as the intensity oscillates in phase with the smoothness of the surface. Using x-ray reflectivity to determine the thin film layer deposition, we grew three films where the x-ray and RHEED oscillations were nearly exactly out of phase and halted deposition at different points in the growth. Pre-growth and post-growth AFM images emphasize the fact that the maxima in RHEED are not a justification for determining layer completion. Work conducted at the Cornell High Energy Synchrotron Source (CHESS) supported by NSF Awards DMR-1332208 and DMR-0936384 and the Cornell Center for Materials Research Shared Facilities are supported through DMR-1120296.

Thin layer chromatography coupled with surface-enhanced Raman scattering as a facile method for on-site quantitative monitoring of chemical reactions.

PubMed

Zhang, Zong-Mian; Liu, Jing-Fu; Liu, Rui; Sun, Jie-Fang; Wei, Guo-Hua

2014-08-05

By coupling surface-enhanced Raman spectroscopy (SERS) with thin layer chromatography (TLC), a facile and powerful method was developed for on-site monitoring the process of chemical reactions. Samples were preseparated on a TLC plate following a common TLC procedure, and then determined by SERS after fabricating a large-area, uniform SERS substrate on the TLC plate by spraying gold nanoparticles (AuNPs). Reproducible and strong SERS signals were obtained with substrates prepared by spraying 42-nm AuNPs at a density of 5.54 × 10(10) N/cm(2) on the TLC plate. The capacity of this TLC-SERS method was evaluated by monitoring a typical Suzuki coupling reaction of phenylboronic acid and 2-bromopyridine as a model. Results showed that this proposed method is able to identify reaction product that is invisible to the naked eye, and distinguish the reactant 2-bromopyridine and product 2-phenylpyridine, which showed almost the same retention factors (R(f)). Under the optimized conditions, the peak area of the characteristic Raman band (755 cm(-1)) of the product 2-phenylpyridine showed a good linear correlation with concentration in the range of 2-200 mg/L (R(2) = 0.9741), the estimated detection limit (1 mg/L 2-phenylpyridine) is much lower than the concentration of the chemicals in the common organic synthesis reaction system, and the product yield determined by the proposed TLC-SERS method agreed very well with that by UPLC-MS/MS. In addition, a new byproduct in the reaction system was found and identified through continuous Raman detection from the point of sample to the solvent front. This facile TLC-SERS method is quick, easy to handle, low-cost, sensitive, and can be exploited in on-site monitoring the processes of chemical reactions, as well as environmental and biological processes.

The experimental design approach to eluotropic strength of 20 solvents in thin-layer chromatography on silica gel.

PubMed

Komsta, Łukasz; Stępkowska, Barbara; Skibiński, Robert

2017-02-03

The eluotropic strength on thin-layer silica plates was investigated for 20 chromatographic grade solvents available in current market. 35 model compounds were used as test subjects in the investigation. The use of modern mixture screening design allowed to estimate each solvent as a separate elution coefficient with an acceptable error of estimation (0.0913 of R M value). Additional bootstrapping technique was used to check the distribution and uncertainty of eluotropic estimates, proving very similar confidence intervals to linear regression. Principal component analysis proved that the only one parameter (mean eluotropic strength) is satisfactory to describe the solvent property, as it explains almost 90% of variance of retention. The obtained eluotropic data can be good appendix to earlier published results and their values can be interpreted in context of R M differences. Copyright © 2017 Elsevier B.V. All rights reserved.

The experimental design approach to eluotropic strength of 20 solvents in thin-layer chromatography on silica gel.

PubMed

Komsta, Łukasz; Stępkowska, Barbara; Skibiński, Robert

2017-01-04

The eluotropic strength on thin-layer silica plates was investigated for 20 chromatographic grade solvents available in current market. 35 model compounds were used as test subjects in the investigation. The use of modern mixture screening design allowed to estimate each solvent as a separate elution coefficient with an acceptable error of estimation (0.0913 of R M value). Additional bootstrapping technique was used to check the distribution and uncertainty of eluotropic estimates, proving very similar confidence intervals to linear regression. Principal component analysis proved that the only one parameter (mean eluotropic strength) is satisfactory to describe the solvent property, as it explains almost 90% of variance of retention. The obtained eluotropic data can be good appendix to earlier published results and their values can be interpreted in context of R M differences. Copyright © 2017 Elsevier B.V. All rights reserved.

Developments of the Physical and Electrical Properties of NiCr and NiCrSi Single-Layer and Bi-Layer Nano-Scale Thin-Film Resistors.

PubMed

Cheng, Huan-Yi; Chen, Ying-Chung; Li, Chi-Lun; Li, Pei-Jou; Houng, Mau-Phon; Yang, Cheng-Fu

2016-02-25

In this study, commercial-grade NiCr (80 wt % Ni, 20 wt % Cr) and NiCrSi (55 wt % Ni, 40 wt % Cr, 5 wt % Si) were used as targets and the sputtering method was used to deposit NiCr and NiCrSi thin films on Al₂O₃ and Si substrates at room temperature under different deposition time. X-ray diffraction patterns showed that the NiCr and NiCrSi thin films were amorphous phase, and the field-effect scanning electronic microscope observations showed that only nano-crystalline grains were revealed on the surfaces of the NiCr and NiCrSi thin films. The log (resistivity) values of the NiCr and NiCrSi thin-film resistors decreased approximately linearly as their thicknesses increased. We found that the value of temperature coefficient of resistance (TCR value) of the NiCr thin-film resistors was positive and that of the NiCrSi thin-film resistors was negative. To investigate these thin-film resistors with a low TCR value, we designed a novel bi-layer structure to fabricate the thin-film resistors via two different stacking methods. The bi-layer structures were created by depositing NiCr for 10 min as the upper (or lower) layer and depositing NiCrSi for 10, 30, or 60 min as the lower (or upper) layer. We aim to show that the stacking method had no apparent effect on the resistivity of the NiCr-NiCrSi bi-layer thin-film resistors but had large effect on the TCR value.

Effect of ZnO buffer layer on phase transition properties of vanadium dioxide thin films

NASA Astrophysics Data System (ADS)

Zhu, Huiqun; Li, Lekang; Li, Chunbo

2016-03-01

VO2 thin films were prepared on ZnO buffer layers by DC magnetron sputtering at room temperature using vanadium target and post annealing at 400 °C. The ZnO buffer layers with different thickness deposited on glass substrates by magnetron sputtering have a high visible and near infrared optical transmittance. The electrical resistivity and the phase transition properties of the VO2/ZnO composite thin films in terms of temperature were investigated. The results showed that the resistivity variation of VO2 thin film with ZnO buffer layer deposited for 35 min was 16 KΩ-cm. The VO2/ZnO composite thin films exhibit a reversible semiconductor-metal phase transition at 48 °C.

Exhaustive thin-layer cyclic voltammetry for absolute multianalyte halide detection.

PubMed

Cuartero, Maria; Crespo, Gastón A; Ghahraman Afshar, Majid; Bakker, Eric

2014-11-18

Water analysis is one of the greatest challenges in the field of environmental analysis. In particular, seawater analysis is often difficult because a large amount of NaCl may mask the determination of other ions, i.e., nutrients, halides, and carbonate species. We demonstrate here the use of thin-layer samples controlled by cyclic voltammetry to analyze water samples for chloride, bromide, and iodide. The fabrication of a microfluidic electrochemical cell based on a Ag/AgX wire (working electrode) inserted into a tubular Nafion membrane is described, which confines the sample solution layer to less than 15 μm. By increasing the applied potential, halide ions present in the thin-layer sample (X(-)) are electrodeposited on the working electrode as AgX, while their respective counterions are transported across the perm-selective membrane to an outer solution. Thin-layer cyclic voltammetry allows us to obtain separated peaks in mixed samples of these three halides, finding a linear relationship between the halide concentration and the corresponding peak area from about 10(-5) to 0.1 M for bromide and iodide and from 10(-4) to 0.6 M for chloride. This technique was successfully applied for the halide analysis in tap, mineral, and river water as well as seawater. The proposed methodology is absolute and potentially calibration-free, as evidenced by an observed 2.5% RSD cell to cell reproducibility and independence from the operating temperature.

Liquid Microjunction Surface Sampling Coupled with High-Pressure Liquid Chromatography-Electrospray Ionization-Mass Spectrometry for Analysis of Drugs and Metabolites in Whole-Body Thin Tissue Sections

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

Kertesz, Vilmos; Van Berkel, Gary J

2010-01-01

In this work, a commercially available autosampler was adapted to perform direct liquid microjunction (LMJ) surface sampling followed by a high-pressure liquid chromatography (HPLC) separation of the extract components and detection with electrospray ionization mass spectrometry (ESI-MS). To illustrate the utility of coupling a separation with this direct liquid extraction based surface sampling approach, four different organs (brain, lung, kidney, and liver) from whole-body thin tissue sections of propranolol dosed and control mice were examined. The parent drug was observed in the chromatograms of the surface sampling extracts from all the organs of the dosed mouse examined. In addition, twomore » isomeric phase II metabolites of propranolol (an aliphatic and an aromatic hydroxypropranolol glucuronide) were observed in the chromatograms of the extracts from lung, kidney, and liver. Confirming the presence of one or the other or both of these glucuronides in the extract from the various organs was not possible without the separation. These drug and metabolite data obtained using the LMJ surface sampling/HPLC-MS method and the results achieved by analyzing similar samples by conventional extraction of the tissues and subsequent HPLC-MS analysis were consistent.« less

Comparison of sampling methods for radiocarbon dating of carbonyls in air samples via accelerator mass spectrometry

NASA Astrophysics Data System (ADS)

Schindler, Matthias; Kretschmer, Wolfgang; Scharf, Andreas; Tschekalinskij, Alexander

2016-05-01

Three new methods to sample and prepare various carbonyl compounds for radiocarbon measurements were developed and tested. Two of these procedures utilized the Strecker synthetic method to form amino acids from carbonyl compounds with either sodium cyanide or trimethylsilyl cyanide. The third procedure used semicarbazide to form crystalline carbazones with the carbonyl compounds. The resulting amino acids and semicarbazones were then separated and purified using thin layer chromatography. The separated compounds were then combusted to CO2 and reduced to graphite to determine 14C content by accelerator mass spectrometry (AMS). All of these methods were also compared with the standard carbonyl compound sampling method wherein a compound is derivatized with 2,4-dinitrophenylhydrazine and then separated by high-performance liquid chromatography (HPLC).

Ultra-thin, single-layer polarization rotator

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

Son, T. V.; Truong, V. V., E-mail: Truong.Vo-Van@Concordia.Ca; Do, P. A.

We demonstrate light polarization control over a broad spectral range by a uniform layer of vanadium dioxide as it undergoes a phase transition from insulator to metal. Changes in refractive indices create unequal phase shifts on s- and p-polarization components of incident light, and rotation of linear polarization shows intensity modulation by a factor of 10{sup 3} when transmitted through polarizers. This makes possible polarization rotation devices as thin as 50 nm that would be activated thermally, optically or electrically.

Metabolomic Strategies Involving Mass Spectrometry Combined with Liquid and Gas Chromatography.

PubMed

Lopes, Aline Soriano; Cruz, Elisa Castañeda Santa; Sussulini, Alessandra; Klassen, Aline

2017-01-01

Amongst all omics sciences, there is no doubt that metabolomics is undergoing the most important growth in the last decade. The advances in analytical techniques and data analysis tools are the main factors that make possible the development and establishment of metabolomics as a significant research field in systems biology. As metabolomic analysis demands high sensitivity for detecting metabolites present in low concentrations in biological samples, high-resolution power for identifying the metabolites and wide dynamic range to detect metabolites with variable concentrations in complex matrices, mass spectrometry is being the most extensively used analytical technique for fulfilling these requirements. Mass spectrometry alone can be used in a metabolomic analysis; however, some issues such as ion suppression may difficultate the quantification/identification of metabolites with lower concentrations or some metabolite classes that do not ionise as well as others. The best choice is coupling separation techniques, such as gas or liquid chromatography, to mass spectrometry, in order to improve the sensitivity and resolution power of the analysis, besides obtaining extra information (retention time) that facilitates the identification of the metabolites, especially when considering untargeted metabolomic strategies. In this chapter, the main aspects of mass spectrometry (MS), liquid chromatography (LC) and gas chromatography (GC) are discussed, and recent clinical applications of LC-MS and GC-MS are also presented.

Thin layered drawing media probed by THz time-domain spectroscopy.

PubMed

Tasseva, J; Taschin, A; Bartolini, P; Striova, J; Fontana, R; Torre, R

2016-12-19

Dry and wet drawing materials were investigated by THz time-domain spectroscopy in transmission mode. Carbon-based and iron-gall inks have been studied, some prepared following ancient recipes and others using current synthetic materials; a commercial ink was studied as well. We measured the THz signals on the thin films of liquid inks deposited on polyethylene pellicles, comparing the results with the thick pellets of dried inks blended with polyethylene powder. This study required the implementation of an accurate experimental method and data analysis procedure able to provide a reliable extraction of the material transmission parameters from a structured sample composed of thin layers, down to a thickness of a few tens of micrometers. THz measurements on thin ink layers enabled the determination of both the absorption and the refractive index in an absolute scale in the 0.1-3 THz range, as well as the layer thickness. THz spectroscopic features of a paper sheet dyed by using one of the iron-gall inks were also investigated. Our results showed that THz time-domain spectroscopy enables the discrimination of various inks on different supports, including the application on paper, together with the proper determination of the absorption coefficients and indices of refraction.

Atomic Force Microscope Mediated Chromatography

NASA Technical Reports Server (NTRS)

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

Optical bandgap of single- and multi-layered amorphous germanium ultra-thin films

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

Liu, Pei; Zaslavsky, Alexander; Longo, Paolo

2016-01-07

Accurate optical methods are required to determine the energy bandgap of amorphous semiconductors and elucidate the role of quantum confinement in nanometer-scale, ultra-thin absorbing layers. Here, we provide a critical comparison between well-established methods that are generally employed to determine the optical bandgap of thin-film amorphous semiconductors, starting from normal-incidence reflectance and transmittance measurements. First, we demonstrate that a more accurate estimate of the optical bandgap can be achieved by using a multiple-reflection interference model. We show that this model generates more reliable results compared to the widely accepted single-pass absorption method. Second, we compare two most representative methods (Taucmore » and Cody plots) that are extensively used to determine the optical bandgap of thin-film amorphous semiconductors starting from the extracted absorption coefficient. Analysis of the experimental absorption data acquired for ultra-thin amorphous germanium (a-Ge) layers demonstrates that the Cody model is able to provide a less ambiguous energy bandgap value. Finally, we apply our proposed method to experimentally determine the optical bandgap of a-Ge/SiO{sub 2} superlattices with single and multiple a-Ge layers down to 2 nm thickness.« less

Comprehensive comparison of liquid chromatography selectivity as provided by two types of liquid chromatography detectors (high resolution mass spectrometry and tandem mass spectrometry): "where is the crossover point?".

PubMed

Kaufmann, A; Butcher, P; Maden, K; Walker, S; Widmer, M

2010-07-12

The selectivity of mass traces obtained by monitoring liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS) and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) was compared. A number of blank extracts (fish, pork kidney, pork liver and honey) were separated by ultra performance liquid chromatography (UPLC). Detected were some 100 dummy transitions respectively dummy exact masses (traces). These dummy masses were the product of a random generator. The range of the permitted masses corresponded to those which are typical for analytes (e.g. veterinary drugs). The large number of monitored dummy traces ensured that endogenous compounds present in the matrix extract, produced a significant number of detectable chromatographic peaks. All obtained chromatographic peaks were integrated and standardized. Standardisation was done by dividing these absolute peak areas by the average response of a set of 7 different veterinary drugs. This permitted a direct comparison between the LC-HRMS and LC-MS/MS data. The data indicated that the selectivity of LC-HRMS exceeds LC-MS/MS, if high resolution mass spectrometry (HRMS) data is recorded with a resolution of 50,000 full width at half maximum (FWHM) and a corresponding mass window. This conclusion was further supported by experimental data (MS/MS based trace analysis), where a false positive finding was observed. An endogenous matrix compound present in honey matrix behaved like a banned nitroimidazole drug. This included identical retention time and two MRM traces, producing an MRM ratio between them, which perfectly matched the ratio observed in the external standard. HRMS measurement clearly resolved the interfering matrix compound and unmasked the false positive MS/MS finding. Copyright 2010 Elsevier B.V. All rights reserved.

Initial formation of calcite crystals in the thin prismatic layer with the periostracum of Pinctada fucata.

PubMed

Suzuki, Michio; Nakayama, Seiji; Nagasawa, Hiromichi; Kogure, Toshihiro

2013-02-01

Although the formation mechanism of calcite crystals in the prismatic layer has been studied well in many previous works, the initial state of calcite formation has not been observed in detail using electron microscopes. In this study, we report that the soft prismatic layer with transparent color (the thin prismatic layer) in the tip of the fresh shell of Pinctada fucata was picked up to observe the early calcification phase. A scanning electron microscope (SEM) image showed that the growth tip of the thin prismatic layer was covered by the periostracum, which was also where the initial formation of calcite crystals began. A cross-section containing the thin calcite crystals in the thin prismatic layer with the periostracum was made using a focused ion beam (FIB) system. In a transmission electron microscope (TEM) observation, the thin calcite crystal (thickness is about 1μm) on the periostracum was found to be a single crystal with the c-axis oriented perpendicular to the shell surface. On the other hand, many aggregated small particles consisting of bassanite crystals were observed in the periostracum suggesting the possibility that not only organic sulfate but also inorganic sulfates exist in the prismatic layer. These discoveries in the early calcification phase of the thin prismatic layer may help to clarify the mechanism of regulating the nucleation and orientation of the calcite crystal in the shell. Copyright © 2012 Elsevier Ltd. All rights reserved.

System and Method for Fabricating Super Conducting Circuitry on Both Sides of an Ultra-Thin Layer

NASA Technical Reports Server (NTRS)

Brown, Ari D. (Inventor); Mikula, Vilem (Inventor)

2017-01-01

A method of fabricating circuitry in a wafer includes depositing a superconducting metal on a silicon on insulator wafer having a handle wafer, coating the wafer with a sacrificial layer and bonding the wafer to a thermally oxide silicon wafer with a first epoxy. The method includes flipping the wafer, thinning the flipped wafer by removing a handle wafer, etching a buried oxide layer, depositing a superconducting layer, bonding the wafer to a thermally oxidized silicon wafer having a handle wafer using an epoxy, flipping the wafer again, thinning the flipped wafer, etching a buried oxide layer from the wafer and etching the sacrificial layer from the wafer. The result is a wafer having superconductive circuitry on both sides of an ultra-thin silicon layer.

Detection of Stimulants and Narcotics by Liquid Chromatography-Tandem Mass Spectrometry and Gas Chromatography-Mass Spectrometry for Sports Doping Control.

PubMed

Ahrens, Brian D; Kucherova, Yulia; Butch, Anthony W

2016-01-01

Sports drug testing laboratories are required to detect several classes of compounds that are prohibited at all times, which include anabolic agents, peptide hormones, growth factors, beta-2 agonists, hormones and metabolic modulators, and diuretics/masking agents. Other classes of compounds such as stimulants, narcotics, cannabinoids, and glucocorticoids are also prohibited, but only when an athlete is in competition. A single class of compounds can contain a large number of prohibited substances and all of the compounds should be detected by the testing procedure. Since there are almost 70 stimulants on the prohibited list it can be a challenge to develop a single screening method that will optimally detect all the compounds. We describe a combined liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) testing method for detection of all the stimulants and narcotics on the World Anti-Doping Agency prohibited list. Urine for LC-MS/MS testing does not require sample pretreatment and is a direct dilute and shoot method. Urine samples for the GC-MS method require a liquid-liquid extraction followed by derivatization with trifluoroacetic anhydride.

Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

PubMed

Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

2016-04-01

In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of toxic compounds in paper-recycling process waters by gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry.

PubMed

Rigol, A; Latorre, A; Lacorte, S; Barceló, D

2002-07-19

Three analytical methods were developed for the determination of toxic compounds in recirculating waters of a paper-recycling industry. Three main groups of compounds were considered: (i) wood extractives originated from the raw material; (ii) biocides added during the production process and (iii) surfactants and other adjuvants present in the formulates of these biocides. Wood extractives considered in this study included fatty and resin acids. They were analysed by liquid-liquid extraction using methyl tert.-butyl ether, followed by gas chromatography-mass spectrometry for previous formation of the respective trimethylsilyl esters. Water samples were also extracted with Oasis HLB (copolymer [poly(divinylbenzene-co-N-vinylpyrrolidone]) solid-phase extraction cartridges of 60 mg and analysed by liquid chromatography-electrospray mass spectrometry for the determination of additives and biocides. Using these two approaches levels up to 15 mg/l for total resin and fatty acids, 5 mg/l for alkylbenzene sulfonates and 2-(thiocyanomethylthio)benzotiazol, 100 microg/l for bisphenol A and 2,2-dibromo-3-nitrilepropionamide, and 300 microg/l for nonylphenol ethoxycarboxylate were detected in process waters at different production treatment stages. These levels are of relevance since poor water quality affects the paper-recycling process, the primary water treatment process and eventually, the environmental water quality.

Developments of the Physical and Electrical Properties of NiCr and NiCrSi Single-Layer and Bi-Layer Nano-Scale Thin-Film Resistors

PubMed Central

Cheng, Huan-Yi; Chen, Ying-Chung; Li, Chi-Lun; Li, Pei-Jou; Houng, Mau-Phon; Yang, Cheng-Fu

2016-01-01

In this study, commercial-grade NiCr (80 wt % Ni, 20 wt % Cr) and NiCrSi (55 wt % Ni, 40 wt % Cr, 5 wt % Si) were used as targets and the sputtering method was used to deposit NiCr and NiCrSi thin films on Al2O3 and Si substrates at room temperature under different deposition time. X-ray diffraction patterns showed that the NiCr and NiCrSi thin films were amorphous phase, and the field-effect scanning electronic microscope observations showed that only nano-crystalline grains were revealed on the surfaces of the NiCr and NiCrSi thin films. The log (resistivity) values of the NiCr and NiCrSi thin-film resistors decreased approximately linearly as their thicknesses increased. We found that the value of temperature coefficient of resistance (TCR value) of the NiCr thin-film resistors was positive and that of the NiCrSi thin-film resistors was negative. To investigate these thin-film resistors with a low TCR value, we designed a novel bi-layer structure to fabricate the thin-film resistors via two different stacking methods. The bi-layer structures were created by depositing NiCr for 10 min as the upper (or lower) layer and depositing NiCrSi for 10, 30, or 60 min as the lower (or upper) layer. We aim to show that the stacking method had no apparent effect on the resistivity of the NiCr-NiCrSi bi-layer thin-film resistors but had large effect on the TCR value. PMID:28344296

The effects of layering in ferroelectric Si-doped HfO{sub 2} thin films

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

Lomenzo, Patrick D.; Nishida, Toshikazu, E-mail: nishida@ufl.edu; Takmeel, Qanit

2014-08-18

Atomic layer deposited Si-doped HfO{sub 2} thin films approximately 10 nm thick are deposited with various Si-dopant concentrations and distributions. The ferroelectric behavior of the HfO{sub 2} thin films are shown to be dependent on both the Si mol. % and the distribution of Si-dopants. Metal-ferroelectric-insulator-semiconductor capacitors are shown to exhibit a tunable remanent polarization through the adjustment of the Si-dopant distribution at a constant Si concentration. Inhomogeneous layering of Si-dopants within the thin films effectively lowers the remanent polarization. A pinched hysteresis loop is observed for higher Si-dopant concentrations and found to be dependent on the Si layering distribution.

Layered ultra-thin coherent structures used as electrical resistors having low-temperature coefficient of resistivity

DOEpatents

Werner, T.R.; Falco, C.M.; Schuller, I.K.

1982-08-31

A thin film resistor having a controlled temperature coefficient of resistance (TCR) ranging from negative to positive degrees kelvin and having relatively high resistivity. The resistor is a multilayer superlattice crystal containing a plurality of alternating, ultra-thin layers of two different metals. TCR is varied by controlling the thickness of the individual layers. The resistor can be readily prepared by methods compatible with thin film circuitry manufacturing techniques.

Thin layer asphaltic concrete density measuring using nuclear gages.

DOT National Transportation Integrated Search

1989-03-01

A Troxler 4640 thin layer nuclear gage was evaluated under field conditions to determine if it would provide improved accuracy of density measurements on asphalt overlays of 1-3/4 and 2 inches in thickness. Statistical analysis shows slightly improve...

Electrospun polyvinyl alcohol ultra-thin layer chromatography of amino acids.

PubMed

Lu, Tian; Olesik, Susan V

2013-01-01

Electrospun polyvinyl alcohol (PVA) ultrathin layer chromatographic (UTLC) plates were fabricated using in situ crosslinking electrospinning technique. The value of these ULTC plates were characterized using the separation of fluorescein isothiocyanate (FITC) labeled amino acids and the separation of amino acids followed visualization using ninhydrin. The in situ crosslinked electrospun PVA plates showed enhanced stability in water and were stable when used for the UTLC study. The selectivity of FITC labeled amino acids on PVA plate was compared with that on commercial Si-Gel plate. The efficiency of the separation varied with analyte concentration, size of capillary analyte applicator, analyte volume, and mat thickness. The concentration of 7mM or less, 50μm i.d. capillary applicator, minimum volume of analyte solution and three-layered mat provides the best efficiency of FITC-labeled amino acids on PVA UTLC plate. The efficiency on PVA plate was greatly improved compared to the efficiency on Si-Gel HPTLC plate. The hydrolysis products of aspartame in diet coke, aspartic acid and phenylalanine, were also successfully analyzed using PVA-UTLC plate. Copyright © 2012 Elsevier B.V. All rights reserved.

Quantitative determination of tilmicosin in canine serum by high performance liquid chromatography-tandem mass spectrometry.

PubMed

Herrera, Michael; Ding, Haiqing; McClanahan, Robert; Owens, Jane G; Hunter, Robert P

2007-09-15

A highly sensitive and quantitative LC/MS/MS assay for the determination of tilmicosin in serum has been developed and validated. For sample preparation, 0.2 mL of canine serum was extracted with 3 mL of methyl tert-butyl ether. The organic layer was transferred to a new vessel and dried under nitrogen. The sample was then reconstituted for analysis by high performance liquid chromatography-tandem mass spectrometry. A Phenomenex Luna C8(2) analytical column was used for the chromatographic separation. The eluent was subsequently introduced to the mass spectrometer by electrospray ionization. A single range was validated for 50-5000 ng/mL for support of toxicokinetic studies. The inter-day relative error (inaccuracy) for the LLOQ samples ranged from -5.5% to 0.3%. The inter-day relative standard deviations (imprecision) at the respective LLOQ levels were < or =10.1%.

Preparation of Ferroelectric Thin Films of Bismuth Layer Structured Compounds

NASA Astrophysics Data System (ADS)

Watanabe, Hitoshi; Mihara, Takashi; Yoshimori, Hiroyuki; Araujo, Carlos

1995-09-01

Ferroelectric thin films of bismuth layer structured compounds, SrBi2Ta2O9, SrBi2Nb2O9, SrBi4Ti4O15 and their solid solutions, were formed onto a sputtered platinum layer on a silicon substrate using spin-on technique and metal-organic decomposition (MOD) method. X-ray diffraction (XRD) analysis and some electrical measurements were performed on the prepared thin films. XRD results of SrBi2(Ta1- x, Nb x)2O9 films (0≤x≤1) showed that niobium ions substitute for tantalum ions in an arbitrary ratio without any change of the layer structure and lattice constants. Furthermore, XRD results of SrBi2 xTa2O9 films (0≤x≤1.5) indicated that the formation of the bismuth layer structure does not always require an accurate bismuth content. The layer structure was formed above 50% of the stoichiometric bismuth content in the general formula. SrBi2(Ta1- x, Nb x)2O9 films with various Ta/Nb ratios have large enough remanent polarization for nonvolatile memory application and have shown high fatigue resistance against 1011 cycles of full switching of the remanent polarization. Mixture films of the three compounds were also investigated.

Pulsed laser deposition of functionalized Mg-Al layered double hydroxide thin films

NASA Astrophysics Data System (ADS)

Vlad, A.; Birjega, R.; Tirca, I.; Matei, A.; Mardare, C. C.; Hassel, A. W.; Nedelcea, A.; Dinescu, M.; Zavoianu, R.

2018-02-01

In this paper, magnesium-aluminium layered double hydroxide (LDH) has been functionalized with sodium dodecyl sulfate (DS) and deposited as thin film by pulsed laser deposition (PLD). Mg, Al-LDH powders were prepared by co-precipitation and used as reference material. Intercalation of DS as an anionic surfactant into the LDHs host layers has been prepared in two ways: co-precipitation (P) and reconstruction (R). DS intercalation occurred in LDH powder via both preparation methods. The films deposited via PLD, in particular at 532 and 1064 nm, preserve the organic intercalated layered structure of the targets prepared from these powders. The results reveal the ability of proposed deposition technique to produce functional composite organo-modified LDHs thin films.

Chemical Composition of Latent Fingerprints by Gas Chromatography-Mass Spectrometry

ERIC Educational Resources Information Center

Hartzell-Baguley, Brittany; Hipp, Rachael E.; Morgan, Neal R.; Morgan, Stephen L.

2007-01-01

An experiment in which gas chromatography-mass spectrometry (GC-MS) is used for latent fingerprint extraction and analysis on glass beads or glass slides is conducted. The results determine that the fingerprint residues are gender dependent.

COMPARATIVE EVALUATION OF GC/MS (GAS CHROMATOGRAPHY/MASS SPECTROMETRY) DATA ANALYSIS PROCESSING

EPA Science Inventory

Mass spectra obtained by fused silica capillary gas chromatography/mass spectrometry/data system (GC/MS/DS) analysis of mixtures of organic chemicals adsorbed on Tenax GC cartridges was subjected to manual and automated interpretative techniques. Synthetic mixtures (85 chemicals ...

Development and evaluation of thin-layer chromatography-digital image-based analysis for the quantitation of the botanical pesticide azadirachtin in agricultural matrixes and commercial formulations: comparison with ELISA.

PubMed

Tanuja, Penmatsa; Venugopal, Namburi; Sashidhar, Rao Beedu

2007-01-01

A simple thin-layer chromatography-digital image-based analytical method has been developed for the quantitation of the botanical pesticide, azadirachtin. The method was validated by analyzing azadirachtin in the spiked food matrixes and processed commercial pesticide formulations, using acidified vanillin reagent as a postchromatographic derivatizing agent. The separated azadirachtin was clearly identified as a green spot. The Rf value was found to be 0.55, which was similar to that of a reference standard. A standard calibration plot was established using a reference standard, based on the linear regression analysis [r2 = 0.996; y = 371.43 + (634.82)x]. The sensitivity of the method was found to be 0.875 microg azadirachtin. Spiking studies conducted at the 1 ppm (microg/g) level in various agricultural matrixes, such as brinjal, tomato, coffee, and cotton seeds, revealed the recoveries of azadirachtin in the range of 67-92%. Azadirachtin content of commercial neem formulations analyzed by the method was in the range of 190-1825 ppm (microg/mL). Further, the present method was compared with an immunoanalytical method enzyme-linked immonosorbent assay developed earlier in our laboratory. Statistical comparison of the 2 methods, using Fischer's F-test, indicated no significant difference in variance, suggesting that both methods are comparable.

Polymerization contraction stress in thin resin composite layers as a function of layer thickness.

PubMed

Alster, D; Feilzer, A J; de Gee, A J; Davidson, C L

1997-05-01

In the present study, the effect of layer thickness on the curing stress in thin resin composite layers was investigated. Since the value of the contraction stress is dependent on the compliance of the measuring equipment (especially for thin films), a method to determine the compliance of the test apparatus was tested. A chemically initiated resin composite (Clearfil F2, Kuraray) was inserted between two sandblasted and silane-coated stainless steel discs in a tensilometer. The curing contraction of the cylindrical samples was continuously counteracted by feedback displacement of the tensilometer crosshead, and the curing stress development was registered. After 20 min, the samples were loaded in tension until fracture. The curing stress was determined for layer thicknesses of 50, 100, 200, 300, 400, 500, 600, 700 microns, 1.4 mm and 2.7 mm. The compliance of the apparatus was calculated with the aid of a non-linear regression analysis, using an equation derived from Hooke's Law as the model. None of the samples fractured due to contraction stress prior to tensile loading. The contraction stress after 20 min decreased from 23.3 +/- 5.3 MPa for the 50 microns layer to 5.5 +/- 0.6 MPa for the 2.7 mm layer. The compliance on the apparatus was 0.029 mm/MPa. A measuring method was developed which was found to be suitable for the determination of axial polymerization contraction stress in this films of chemically initiated resin composites. The method makes it possible to estimate the stress levels that occur in resin composite films in the clinical situation.

Online Hydrophobic Interaction Chromatography-Mass Spectrometry for the Analysis of Intact Monoclonal Antibodies.

PubMed

Chen, Bifan; Lin, Ziqing; Alpert, Andrew J; Fu, Cexiong; Zhang, Qunying; Pritts, Wayne A; Ge, Ying

2018-06-19

Therapeutic monoclonal antibodies (mAbs) are an important class of drugs for a wide spectrum of human diseases. Liquid chromatography (LC) coupled to mass spectrometry (MS) is one of the techniques in the forefront for comprehensive characterization of analytical attributes of mAbs. Among various protein chromatography modes, hydrophobic interaction chromatography (HIC) is a popular offline nondenaturing separation technique utilized to purify and analyze mAbs, typically with the use of non-MS-compatible mobile phases. Herein we demonstrate for the first time, the application of direct HIC-MS and HIC-tandem MS (MS/MS) with electron capture dissociation (ECD) for analyzing intact mAbs on quadrupole-time-of-flight (Q-TOF) and Fourier transform ion cyclotron resonance (FTICR) mass spectrometers, respectively. Our method allows for rapid determination of relative hydrophobicity, intact masses, and glycosylation profiles of mAbs as well as sequence and structural characterization of the complementarity-determining regions in an online configuration.

Characterization of crude oil biomarkers using comprehensive two-dimensional gas chromatography coupled to tandem mass spectrometry.

PubMed

Mogollón, Noroska Gabriela Salazar; Prata, Paloma Santana; Dos Reis, Jadson Zeni; Neto, Eugênio Vaz Dos Santos; Augusto, Fabio

2016-09-01

Oil samples from Recôncavo basin (NE Brazil), previously analyzed by traditional techniques such as gas chromatography coupled to tandem mass spectrometry, were evaluated using comprehensive two-dimensional gas chromatography coupled to quadrupole mass spectrometry and comprehensive two-dimensional gas chromatography coupled to tandem mass spectrometry along with simplified methods of samples preparation to evaluate the differences and advantages of these analytical techniques to better understand the development of the organic matter in this basin without altering the normal distribution of the compounds in the samples. As a result, the geochemical parameters calculated by comprehensive two-dimensional gas chromatography coupled to tandem mass spectrometry described better the origin, maturity, and biodegradation of both samples probably by increased selectivity, resolution, and sensitivity inherent of the multidimensional technique. Additionally, the detection of the compounds such as, the C(14α-) homo-26-nor-17α-hopane series, diamoretanes, nor-spergulanes, C19 -C26 A-nor-steranes and 4α-methylsteranes resolved and detected by comprehensive two-dimensional gas chromatography coupled to tandem mass spectrometry were key to classify and differentiate these lacustrine samples according to their maturity and deposition conditions. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Growth of <111>-oriented Cu layer on thin TaWN films

NASA Astrophysics Data System (ADS)

Takeyama, Mayumi B.; Sato, Masaru

2017-07-01

In this study, we examine the growth of a <111>-oriented Cu layer on a thin TaWN ternary alloy barrier for good electromigration reliability. The strongly preferentially oriented Cu(111) layer is observed on a thin TaWN barrier even in the as-deposited Cu (100 nm)/TaWN (5 nm)/Si system. Also, this system tolerates annealing at 700 °C for 1 h without silicide reaction. It is revealed that the TaWN film is one of the excellent barriers with thermal stability and low resistivity. Simultaneously, the TaWN film is a candidate for a superior underlying material to achieve the Cu(111) preferential orientation.

Bi-layer Channel AZO/ZnO Thin Film Transistors Fabricated by Atomic Layer Deposition Technique

NASA Astrophysics Data System (ADS)

Li, Huijin; Han, Dedong; Liu, Liqiao; Dong, Junchen; Cui, Guodong; Zhang, Shengdong; Zhang, Xing; Wang, Yi

2017-03-01

This letter demonstrates bi-layer channel Al-doped ZnO/ZnO thin film transistors (AZO/ZnO TFTs) via atomic layer deposition process at a relatively low temperature. The effects of annealing in oxygen atmosphere at different temperatures have also been investigated. The ALD bi-layer channel AZO/ZnO TFTs annealed in dry O2 at 300 °C exhibit a low leakage current of 2.5 × 10-13A, I on/ I off ratio of 1.4 × 107, subthreshold swing (SS) of 0.23 V/decade, and high transmittance. The enhanced performance obtained from the bi-layer channel AZO/ZnO TFT devices is explained by the inserted AZO front channel layer playing the role of the mobility booster.

Copper Benzenetricarboxylate Metal-Organic Framework Nucleation Mechanisms on Metal Oxide Powders and Thin Films formed by Atomic Layer Deposition.

PubMed

Lemaire, Paul C; Zhao, Junjie; Williams, Philip S; Walls, Howard J; Shepherd, Sarah D; Losego, Mark D; Peterson, Gregory W; Parsons, Gregory N

2016-04-13

Chemically functional microporous metal-organic framework (MOF) crystals are attractive for filtration and gas storage applications, and recent results show that they can be immobilized on high surface area substrates, such as fiber mats. However, fundamental knowledge is still lacking regarding initial key reaction steps in thin film MOF nucleation and growth. We find that thin inorganic nucleation layers formed by atomic layer deposition (ALD) can promote solvothermal growth of copper benzenetricarboxylate MOF (Cu-BTC) on various substrate surfaces. The nature of the ALD material affects the MOF nucleation time, crystal size and morphology, and the resulting MOF surface area per unit mass. To understand MOF nucleation mechanisms, we investigate detailed Cu-BTC MOF nucleation behavior on metal oxide powders and Al2O3, ZnO, and TiO2 layers formed by ALD on polypropylene substrates. Studying both combined and sequential MOF reactant exposure conditions, we find that during solvothermal synthesis ALD metal oxides can react with the MOF metal precursor to form double hydroxy salts that can further convert to Cu-BTC MOF. The acidic organic linker can also etch or react with the surface to form MOF from an oxide metal source, which can also function as a nucleation agent for Cu-BTC in the mixed solvothermal solution. We discuss the implications of these results for better controlled thin film MOF nucleation and growth.

Quantitative Analysis of Tetramethylenedisulfotetramine ("Tetramine") Spiked into Beverages by Liquid Chromatography Tandem Mass Spectrometry with Validation by Gas Chromatography Mass Spectrometry

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

Owens, J; Hok, S; Alcaraz, A

Tetramethylenedisulfotetramine, commonly known as tetramine, is a highly neurotoxic rodenticide (human oral LD{sub 50} = 0.1 mg/kg) used in hundreds of deliberate food poisoning events in China. Here we describe a method for quantitation of tetramine spiked into beverages, including milk, juice, tea, cola, and water and cleaned up by C8 solid phase extraction and liquid-liquid extraction. Quantitation by high performance liquid chromatography tandem mass spectrometry (LC/MS/MS) was based upon fragmentation of m/z 347 to m/z 268. The method was validated by gas chromatography mass spectrometry (GC/MS) operated in SIM mode for ions m/z 212, 240, and 360. The limitmore » of quantitation was 0.10 {micro}g/mL by LC/MS/MS versus 0.15 {micro}g/mL for GC/MS. Fortifications of the beverages at 2.5 {micro}g/mL and 0.25 {micro}g/mL were recovered ranging from 73-128% by liquid-liquid extraction for GC/MS analysis, 13-96% by SPE and 10-101% by liquid-liquid extraction for LC/MS/MS analysis.« less

Precise Control of the Number of Layers of Graphene by Picosecond Laser Thinning.

PubMed

Lin, Zhe; Ye, Xiaohui; Han, Jinpeng; Chen, Qiao; Fan, Peixun; Zhang, Hongjun; Xie, Dan; Zhu, Hongwei; Zhong, Minlin

2015-06-26

The properties of graphene can vary as a function of the number of layers (NOL). Controlling the NOL in large area graphene is still challenging. In this work, we demonstrate a picosecond (ps) laser thinning removal of graphene layers from multi-layered graphene to obtain desired NOL when appropriate pulse threshold energy is adopted. The thinning process is conducted in atmosphere without any coating and it is applicable for graphene films on arbitrary substrates. This method provides many advantages such as one-step process, non-contact operation, substrate and environment-friendly, and patternable, which will enable its potential applications in the manufacturing of graphene-based electronic devices.

Precise Control of the Number of Layers of Graphene by Picosecond Laser Thinning

NASA Astrophysics Data System (ADS)

Lin, Zhe; Ye, Xiaohui; Han, Jinpeng; Chen, Qiao; Fan, Peixun; Zhang, Hongjun; Xie, Dan; Zhu, Hongwei; Zhong, Minlin

2015-06-01

The properties of graphene can vary as a function of the number of layers (NOL). Controlling the NOL in large area graphene is still challenging. In this work, we demonstrate a picosecond (ps) laser thinning removal of graphene layers from multi-layered graphene to obtain desired NOL when appropriate pulse threshold energy is adopted. The thinning process is conducted in atmosphere without any coating and it is applicable for graphene films on arbitrary substrates. This method provides many advantages such as one-step process, non-contact operation, substrate and environment-friendly, and patternable, which will enable its potential applications in the manufacturing of graphene-based electronic devices.

Bi-layer Channel AZO/ZnO Thin Film Transistors Fabricated by Atomic Layer Deposition Technique.

PubMed

Li, Huijin; Han, Dedong; Liu, Liqiao; Dong, Junchen; Cui, Guodong; Zhang, Shengdong; Zhang, Xing; Wang, Yi

2017-12-01

This letter demonstrates bi-layer channel Al-doped ZnO/ZnO thin film transistors (AZO/ZnO TFTs) via atomic layer deposition process at a relatively low temperature. The effects of annealing in oxygen atmosphere at different temperatures have also been investigated. The ALD bi-layer channel AZO/ZnO TFTs annealed in dry O 2 at 300 °C exhibit a low leakage current of 2.5 × 10 -13 A, I on /I off ratio of 1.4 × 10 7 , subthreshold swing (SS) of 0.23 V/decade, and high transmittance. The enhanced performance obtained from the bi-layer channel AZO/ZnO TFT devices is explained by the inserted AZO front channel layer playing the role of the mobility booster.

Liquid Chromatography-Tandem Mass Spectrometry: An Emerging Technology in the Toxicology Laboratory.

PubMed

Zhang, Yan Victoria; Wei, Bin; Zhu, Yu; Zhang, Yanhua; Bluth, Martin H

2016-12-01

In the last decade, liquid chromatography-tandem mass spectrometry (LC-MS/MS) has seen enormous growth in routine toxicology laboratories. LC-MS/MS offers significant advantages over other traditional testing, such as immunoassay and gas chromatography-mass spectrometry methodologies. Major strengths of LC-MS/MS include improvement in specificity, flexibility, and sample throughput when compared with other technologies. Here, the basic principles of LC-MS/MS technology are reviewed, followed by advantages and disadvantages of this technology compared with other traditional techniques. In addition, toxicology applications of LC-MS/MS for simultaneous detection of large panels of analytes are presented. Copyright © 2016 Elsevier Inc. All rights reserved.

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

ERIC Educational Resources Information Center

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…

Layer-by-layer modification of thin-film metal-semiconductor multilayers with ultrashort laser pulses

NASA Astrophysics Data System (ADS)

Romashevskiy, S. A.; Tsygankov, P. A.; Ashitkov, S. I.; Agranat, M. B.

2018-05-01

The surface modifications in a multilayer thin-film structure (50-nm alternating layers of Si and Al) induced by a single Gaussian-shaped femtosecond laser pulse (350 fs, 1028 nm) in the air are investigated by means of atomic-force microscopy (AFM), scanning electron microscopy (SEM), and optical microscopy (OM). Depending on the laser fluence, various modifications of nanometer-scale metal and semiconductor layers, including localized formation of silicon/aluminum nanofoams and layer-by-layer removal, are found. While the nanofoams with cell sizes in the range of tens to hundreds of nanometers are produced only in the two top layers, layer-by-layer removal is observed for the four top layers under single pulse irradiation. The 50-nm films of the multilayer structure are found to be separated at their interfaces, resulting in a selective removal of several top layers (up to 4) in the form of step-like (concentric) craters. The observed phenomenon is associated with a thermo-mechanical ablation mechanism that results in splitting off at film-film interface, where the adhesion force is less than the bulk strength of the used materials, revealing linear dependence of threshold fluences on the film thickness.

GLC analysis of base composition of RNA and DNA hydrolysates

NASA Technical Reports Server (NTRS)

Lakings, D. B.; Gehreke, C. W.

1971-01-01

Various methods used for the analysis of the base composition of RNA and DNA hydrolysates are presented. The methods discussed are: (1) ion-exchange chromatography, (2) paper chromatography, (3) paper electrophoresis, (4) thin layer chromatography, (5) paper chromatography and time of flight mass spectrometry, and (6) gas-liquid chromatography. The equipment required and the conditions for obtaining the best results with each method are described.

Prostate cell membrane chromatography-liquid chromatography-mass spectrometry for screening of active constituents from Uncaria rhynchophylla.

PubMed

He, Jianyu; Han, Shengli; Yang, Fangfang; Zhou, Nan; Wang, Sicen

2013-01-01

Uncaria rhynchophylla is a traditional Chinese medicinal herb used to treat hypertension and convulsive disorders such as epilepsy. Rat prostate cell membrane chromatography combined with liquid chromatography-mass spectrometry (LC-MS) was used to identify active constituents from U. rhynchophylla extracts. Four compounds (corynoxeine, isorhynchophylline, isocorynoxeine and rhynchophylline) were discovered. Competitive binding assay results indicated that the four compounds were in direct competition at a single common binding site and interacted with α1A adrenergic receptors (α1A-AR) in a manner similar to tamsulosin. Affinity constant values of the four compounds binding with α1A-AR were also measured using rat prostate cell membrane chromatography (CMC). Finally, their pharmacodynamic effects were tested on rat caudal arteries. This CMC combined LC-MS system offers a means of drug discovery by screening natural medicinal herbs for new pharmacologically active molecules targeting specific receptors.

Planar solid phase extraction clean-up for pesticide residue analysis in tea by liquid chromatography-mass spectrometry.

PubMed

Oellig, Claudia; Schwack, Wolfgang

2012-10-19

Efficient clean-up is indispensable for preventing matrix effects in multi-residue analysis of pesticides in food by liquid and gas chromatography (LC and GC) coupled to mass spectrometry (MS). High-throughput planar solid phase extraction (HTpSPE) was recently introduced as a new clean-up concept in residue analysis of pesticides in fruit and vegetables (C. Oellig, W. Schwack, 2011 [45]). 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. As rather challenging matrices, tea samples were chosen in this study. Besides chlorophylls and polyphenols, high amount of caffeine is co-extracted resulting in strong matrix effects both in LC-MS and GC-MS. The former HTpSPE procedure was adapted to initial extracts of green and black tea resulting in colorless extracts nearly free of matrix effects and interferences, as shown for seven chemically representative pesticides (acetamiprid, penconazole, azoxystrobin, chlorpyrifos, pirimicarb, fenarimol, and mepanipyrim). LC-MS/MS calibration curves obtained in the range of 0.002-0.5 mg/kg from matrix-matched standards and solvent standards were nearly identical and demonstrated the effectiveness of clean-up by HTpSPE. Mean recoveries determined by LC-MS/MS against solvent standards at spiking levels of 0.01 and 0.1 mg/kg ranged between 72 and 114% with relative standard deviations (RSDs) of 0.7-4.7% (n=4), while LC-MS measurements of tea samples spiked at 1 mg/kg provided recoveries of 81-104% with RSDs of 1.2-4.9% (n=6). Using LC-MS/MS, the method showed high sensitivity with signal-to-noise ratios>10 for concentrations below 0.002 mg/kg. HTpSPE of one sample was done in a few minutes, while numerous samples were cleaned in parallel at minimal costs with very low sample and solvent consumption. Copyright © 2012 Elsevier B.V. All rights reserved.

Atomically thin gallium layers from solid-melt exfoliation

PubMed Central

Kochat, Vidya; Samanta, Atanu; Zhang, Yuan; Bhowmick, Sanjit; Manimunda, Praveena; Asif, Syed Asif S.; Stender, Anthony S.; Vajtai, Robert; Singh, Abhishek K.; Tiwary, Chandra S.; Ajayan, Pulickel M.

2018-01-01

Among the large number of promising two-dimensional (2D) atomic layer crystals, true metallic layers are rare. Using combined theoretical and experimental approaches, we report on the stability and successful exfoliation of atomically thin “gallenene” sheets on a silicon substrate, which has two distinct atomic arrangements along crystallographic twin directions of the parent α-gallium. With a weak interface between solid and molten phases of gallium, a solid-melt interface exfoliation technique is developed to extract these layers. Phonon dispersion calculations show that gallenene can be stabilized with bulk gallium lattice parameters. The electronic band structure of gallenene shows a combination of partially filled Dirac cone and the nonlinear dispersive band near the Fermi level, suggesting that gallenene should behave as a metallic layer. Furthermore, it is observed that the strong interaction of gallenene with other 2D semiconductors induces semiconducting to metallic phase transitions in the latter, paving the way for using gallenene as promising metallic contacts in 2D devices. PMID:29536039

Applicability of preparative overpressured layer chromatography and direct bioautography in search of antibacterial chamomile compounds.

PubMed

Móricz, Agnes M; Ott, Péter G; Alberti, Agnes; Böszörményi, Andrea; Lemberkovics, Eva; Szoke, Eva; Kéry, Agnes; Mincsovics, Emil

2013-01-01

In situ sample preparation and preparative overpressured layer chromatography (OPLC) fractionation on a 0.5 mm thick adsorbent layer of chamomile flower methanol extract prepurified by conventional gravitation accelerated column chromatography were applied in searching for bioactive components. Sample cleanup in situ on the adsorbent layer subsequent to sample application was performed using mobile phase flow in the opposite direction (the input and output of the eluent was exchanged). The antibacterial effect of the fractions obtained from the stepwise gradient OPLC separation with the flow in the normal direction was evaluated by direct bioautography against two Gram-negative bacteria: the luminescence gene tagged plant pathogenic Pseudomonas syringae pv. maculicola, and the naturally luminescent marine bacterium Vibrio fischeri. The fractions having strong activity were analyzed by SPME-GC/MS and HPLC/MS/MS. Mainly essential oil components, coumarins, flavonoids, phenolic acids, and fatty acids were tentatively identified in the fractions.

Layer-controllable graphene by plasma thinning and post-annealing

NASA Astrophysics Data System (ADS)

Zhang, Lufang; Feng, Shaopeng; Xiao, Shaoqing; Shen, Gang; Zhang, Xiumei; Nan, Haiyan; Gu, Xiaofeng; Ostrikov, Kostya (Ken)

2018-05-01

The electronic structure of graphene depends crucially on its layer number and therefore engineering the number of graphene's atomic stacking layers is of great importance for the preparation of graphene-based devices. In this paper, we demonstrated a relatively less invasive, high-throughput and uniform large-area plasma thinning of graphene based on direct bombardment effect of fast-moving ionic hydrogen or argon species. Any desired number of graphene layers including trilayer, bilayer and monolayer can be obtained. Structural changes of graphene layers are studied by optical microscopy, Raman spectroscopy and atomic force microscopy. Post annealing is adopted to self-heal the lattice defects induced by the ion bombardment effect. This plasma etching technique is efficient and compatible with semiconductor manufacturing processes, and may find important applications for graphene-based device fabrication.

Column chromatography as a useful step in purification of diatom pigments.

PubMed

Tokarek, Wiktor; Listwan, Stanisław; Pagacz, Joanna; Leśniak, Piotr; Latowski, Dariusz

2016-01-01

Fucoxanthin, diadinoxanthin and diatoxanthin are carotenoids found in brown algae and most other heterokonts. These pigments are involved in photosynthetic and photoprotective reactions, and they have many potential health benefits. They can be extracted from diatom Phaeodactylum tricornutum by sonication, extraction with chloroform : methanol and preparative thin layer chromatography. We assessed the utility of an additional column chromatography step in purification of these pigments. This novel addition to the isolation protocol increased the purity of fucoxanthin and allowed for concentration of diadinoxanthin and diatoxanthin before HPLC separation. The enhanced protocol is useful for obtaining high purity pigments for biochemical studies.

High performance thin film transistor with ZnO channel layer deposited by DC magnetron sputtering.

PubMed

Moon, Yeon-Keon; Moon, Dae-Yong; Lee, Sang-Ho; Jeong, Chang-Oh; Park, Jong-Wan

2008-09-01

Research in large area electronics, especially for low-temperature plastic substrates, focuses commonly on limitations of the semiconductor in thin film transistors (TFTs), in particular its low mobility. ZnO is an emerging example of a semiconductor material for TFTs that can have high mobility, while a-Si and organic semiconductors have low mobility (<1 cm2/Vs). ZnO-based TFTs have achieved high mobility, along with low-voltage operation low off-state current, and low gate leakage current. In general, ZnO thin films for the channel layer of TFTs are deposited with RF magnetron sputtering methods. On the other hand, we studied ZnO thin films deposited with DC magnetron sputtering for the channel layer of TFTs. After analyzing the basic physical and chemical properties of ZnO thin films, we fabricated a TFT-unit cell using ZnO thin films for the channel layer. The field effect mobility (micro(sat)) of 1.8 cm2/Vs and threshold voltage (Vth) of -0.7 V were obtained.

Thin film photovoltaic devices with a minimally conductive buffer layer

DOEpatents

Barnes, Teresa M.; Burst, James

2016-11-15

A thin film photovoltaic device (100) with a tunable, minimally conductive buffer (128) layer is provided. The photovoltaic device (100) may include a back contact (150), a transparent front contact stack (120), and an absorber (140) positioned between the front contact stack (120) and the back contact (150). The front contact stack (120) may include a low resistivity transparent conductive oxide (TCO) layer (124) and a buffer layer (128) that is proximate to the absorber layer (140). The photovoltaic device (100) may also include a window layer (130) between the buffer layer (128) and the absorber (140). In some cases, the buffer layer (128) is minimally conductive, with its resistivity being tunable, and the buffer layer (128) may be formed as an alloy from a host oxide and a high-permittivity oxide. The high-permittivity oxide may further be chosen to have a bandgap greater than the host oxide.

High-resolution liquid chromatography/electrospray ionization time-of-flight mass spectrometry combined with liquid chromatography/electrospray ionization tandem mass spectrometry to identify polyphenols from grape antioxidant dietary fiber.

PubMed

Touriño, Sonia; Fuguet, Elisabet; Jáuregui, Olga; Saura-Calixto, Fulgencio; Cascante, Marta; Torres, Josep Lluís

2008-11-01

Grape antioxidant dietary fiber (GADF) is a dietary supplement that combines the benefits of both fiber and antioxidants that help prevent cancer and cardiovascular diseases. The antioxidant polyphenolic components in GADF probably help prevent cancer in the digestive tract, where they are bioavailable. Mass spectrometry coupled to liquid chromatography is a powerful tool for the analysis of complex plant derivatives such as GADF. We use a combination of MS techniques, namely liquid chromatography/electrospray ionization time-of-flight mass spectrometry (LC/ESI-TOF-MS) and liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) on a triple quadrupole, for the identification of the polyphenolic constituents of the soluble fraction of GADF. First, we separated the mixture into four fractions which were tested for phenolic constituents using the TOF system in the full scan mode. The high sensitivity and resolution of the TOF detector over the triple quadrupole facilitate the preliminary characterization of the fractions. Then we used LC/ESI-MS/MS to identify the individual phenols through MS/MS experiments (product ion scan, neutral loss scan, precursor ion scan). Finally, most of the identities were unequivocally confirmed by accurate mass measurements on the TOF spectrometer. LC/ESI-TOF-MS combined with MS/MS correctly identifies the bioactive polyphenolic components from the soluble fraction of GADF. High-resolution TOF-MS is particularly useful for identifying the structure of compounds with the same LC/ESI-MS/MS fragmentation patterns.

Mixed-mode chromatography/isotope ratio mass spectrometry.

PubMed

McCullagh, James S O

2010-03-15

Liquid chromatography coupled to molecular mass spectrometry (LC/MS) has been a standard technique since the early 1970s but liquid chromatography coupled to high-precision isotope ratio mass spectrometry (LC/IRMS) has only been available commercially since 2004. This development has, for the first time, enabled natural abundance and low enrichment delta(13)C measurements to be applied to individual analytes in aqueous mixtures creating new opportunities for IRMS applications, particularly for the isotopic study of biological molecules. A growing number of applications have been published in a range of areas including amino acid metabolism, carbohydrates studies, quantification of cellular and plasma metabolites, dietary tracer and nucleic acid studies. There is strong potential to extend these to new compounds and complex matrices but several challenges face the development of LC/IRMS methods. To achieve accurate isotopic measurements, HPLC separations must provide baseline-resolution between analyte peaks; however, the design of current liquid interfaces places severe restrictions on compatible flow rates and in particular mobile phase compositions. These create a significant challenge on which reports associated with LC/IRMS have not previously focused. Accordingly, this paper will address aspects of chromatography in the context of LC/IRMS, in particular focusing on mixed-mode separations and their benefits in light of these restrictions. It aims to provide an overview of mixed-mode stationary phases and of ways to improve high aqueous separations through manipulation of parameters such as column length, temperature and mobile phase pH. The results of several practical experiments are given using proteogenic amino acids and nucleosides both of which are of noted importance in the LC/IRMS literature. This communication aims to demonstrate that mixed-mode stationary phases provide a flexible approach given the constraints of LC/IRMS interface design and acts as a

Comprehensive lipidomic analysis of human plasma using multidimensional liquid- and gas-phase separations: Two-dimensional liquid chromatography-mass spectrometry vs. liquid chromatography-trapped-ion-mobility-mass spectrometry.

PubMed

Baglai, Anna; Gargano, Andrea F G; Jordens, Jan; Mengerink, Ynze; Honing, Maarten; van der Wal, Sjoerd; Schoenmakers, Peter J

2017-12-29

Recent advancements in separation science have resulted in the commercialization of multidimensional separation systems that provide higher peak capacities and, hence, enable a more-detailed characterization of complex mixtures. In particular, two powerful analytical tools are increasingly used by analytical scientists, namely online comprehensive two-dimensional liquid chromatography (LC×LC, having a second-dimension separation in the liquid phase) and liquid chromatography-ion mobility-spectrometry (LC-IMS, second dimension separation in the gas phase). The goal of the current study was a general assessment of the liquid-chromatography-trapped-ion-mobility-mass spectrometry (LC-TIMS-MS) and comprehensive two-dimensional liquid chromatography-mass spectrometry (LC×LC-MS) platforms for untargeted lipid mapping in human plasma. For the first time trapped-ion-mobility spectrometry (TIMS) was employed for the separation of the major lipid classes and ion-mobility-derived collision-cross-section values were determined for a number of lipid standards. The general effects of a number of influencing parameters have been inspected and possible directions for improvements are discussed. We aimed to provide a general indication and practical guidelines for the analyst to choose an efficient multidimensional separation platform according to the particular requirements of the application. Analysis time, orthogonality, peak capacity, and an indicative measure for the resolving power are discussed as main characteristics for multidimensional separation systems. Copyright © 2017 Elsevier B.V. All rights reserved.

Recent Advance in Liquid Chromatography/Mass Spectrometry Techniques for Environmental Analysis in Japan

PubMed Central

Suzuki, Shigeru

2014-01-01

The techniques and measurement methods developed in the Environmental Survey and Monitoring of Chemicals by Japan’s Ministry of the Environment, as well as a large amount of knowledge archived in the survey, have led to the advancement of environmental analysis. Recently, technologies such as non-target liquid chromatography/high resolution mass spectrometry and liquid chromatography with micro bore column have further developed the field. Here, the general strategy of a method developed for the liquid chromatography/mass spectrometry (LC/MS) analysis of environmental chemicals with a brief description is presented. Also, a non-target analysis for the identification of environmental pollutants using a provisional fragment database and “MsMsFilter,” an elemental composition elucidation tool, is presented. This analytical method is shown to be highly effective in the identification of a model chemical, the pesticide Bendiocarb. Our improved micro-liquid chromatography injection system showed substantially enhanced sensitivity to perfluoroalkyl substances, with peak areas 32–71 times larger than those observed in conventional LC/MS. PMID:26819891

Advances in native high-performance liquid chromatography and intact mass spectrometry for the characterization of biopharmaceutical products.

PubMed

Tassi, Marco; De Vos, Jelle; Chatterjee, Sneha; Sobott, Frank; Bones, Jonathan; Eeltink, Sebastiaan

2018-01-01

The characterization of biotherapeutics represents a major analytical challenge. This review discusses the current state-of-the-art in analytical technologies to profile biopharma products under native conditions, i.e., the protein three dimensional conformation is maintained during liquid chromatographic analysis. Native liquid-chromatographic modes that are discussed include aqueous size-exclusion chromatography, hydrophobic interaction chromatography, and ion-exchange chromatography. Infusion conditions and the possibilities and limitations to hyphenate native liquid chromatography to mass spectrometry are discussed. Furthermore, the applicability of native liquid-chromatography methods and intact mass spectrometry analysis for the characterization of monoclonal antibodies and antibody-drug conjugates is discussed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Photo-EMF sensitivity of porous silicon thin layer-crystalline silicon heterojunction to ammonia adsorption.

PubMed

Vashpanov, Yuriy; Jung, Jae Il; Kwack, Kae Dal

2011-01-01

A new method of using photo-electromotive force in detecting gas and controlling sensitivity is proposed. Photo-electromotive force on the heterojunction between porous silicon thin layer and crystalline silicon wafer depends on the concentration of ammonia in the measurement chamber. A porous silicon thin layer was formed by electrochemical etching on p-type silicon wafer. A gas and light transparent electrical contact was manufactured to this porous layer. Photo-EMF sensitivity corresponding to ammonia concentration in the range from 10 ppm to 1,000 ppm can be maximized by controlling the intensity of illumination light.

Carbohydrate profiling of bacteria by gas chromatography-mass spectrometry and their trace detection in complex matrices by gas chromatography-tandem mass spectrometry.

PubMed

Fox, A

1999-05-28

Bacterial cellular polysaccharides are composed of a variety of sugar monomers. These sugars serve as chemical markers to identify specific species or genera or to determine their physiological status. Some of these markers can also be used for trace detection of bacteria or their constituents in complex clinical or environmental matrices. Analyses are performed, in our hands, employing hydrolysis followed by the alditol acetate derivatization procedure. Substantial improvements have been made to sample preparation including simplification and computer-controlled automation. For characterization of whole cell bacterial hydrolysates, sugars are analyzed by gas chromatography-mass spectrometry (GC-MS). Simple chromatograms are generated using selected ion monitoring (SIM). Using total ion GC-MS, sugars can be readily identified. In more complex clinical and environmental samples, markers for bacteria are present at sufficiently low concentrations that more advanced instrumentation, gas chromatography-tandem mass spectrometry (GC-MS-MS), is preferred for optimal analysis. Using multiple reaction monitoring, MS-MS is used (replacing more conventional SIM) to ignore extraneous chromatographic peaks. Triple quadrupole and ion trap GC-MS-MS instruments have both been used successfully. Absolute chemical identification of sugar markers at trace levels is achieved, using MS-MS, by the product spectrum.

Modified Back Contact Interface of CZTSe Thin Film Solar Cells: Elimination of Double Layer Distribution in Absorber Layer

PubMed Central

Zhang, Zhaojing; Yao, Liyong; Bi, Jinlian; Gao, Shoushuai; Gao, Qing; Jeng, Ming‐Jer; Sun, Guozhong; Zhou, Zhiqiang; He, Qing; Sun, Yun

2017-01-01

Abstract Double layer distribution exists in Cu2SnZnSe4 (CZTSe) thin films prepared by selenizing the metallic precursors, which will degrade the back contact of Mo substrate to absorber layer and thus suppressing the performance of solar cell. In this work, the double‐layer distribution of CZTSe film is eliminated entirely and the formation of MoSe2 interfacial layer is inhibited successfully. CZTSe film is prepared by selenizing the precursor deposited by electrodeposition method under Se and SnSex mixed atmosphere. It is found that the insufficient reaction between ZnSe and Cu‐Sn‐Se phases in the bottom of the film is the reason why the double layer distribution of CZTSe film is formed. By increasing Sn content in the metallic precursor, thus making up the loss of Sn because of the decomposition of CZTSe and facilitate the diffusion of liquid Cu2Se, the double layer distribution is eliminated entirely. The crystallization of the formed thin film is dense and the grains go through the entire film without voids. And there is no obvious MoSe2 layer formed between CZTSe and Mo. As a consequence, the series resistance of the solar cell reduces significantly to 0.14 Ω cm2 and a CZTSe solar cell with efficiency of 7.2% is fabricated. PMID:29610727

Modified Back Contact Interface of CZTSe Thin Film Solar Cells: Elimination of Double Layer Distribution in Absorber Layer.

PubMed

Zhang, Zhaojing; Yao, Liyong; Zhang, Yi; Ao, Jianping; Bi, Jinlian; Gao, Shoushuai; Gao, Qing; Jeng, Ming-Jer; Sun, Guozhong; Zhou, Zhiqiang; He, Qing; Sun, Yun

2018-02-01

Double layer distribution exists in Cu 2 SnZnSe 4 (CZTSe) thin films prepared by selenizing the metallic precursors, which will degrade the back contact of Mo substrate to absorber layer and thus suppressing the performance of solar cell. In this work, the double-layer distribution of CZTSe film is eliminated entirely and the formation of MoSe 2 interfacial layer is inhibited successfully. CZTSe film is prepared by selenizing the precursor deposited by electrodeposition method under Se and SnSe x mixed atmosphere. It is found that the insufficient reaction between ZnSe and Cu-Sn-Se phases in the bottom of the film is the reason why the double layer distribution of CZTSe film is formed. By increasing Sn content in the metallic precursor, thus making up the loss of Sn because of the decomposition of CZTSe and facilitate the diffusion of liquid Cu 2 Se, the double layer distribution is eliminated entirely. The crystallization of the formed thin film is dense and the grains go through the entire film without voids. And there is no obvious MoSe 2 layer formed between CZTSe and Mo. As a consequence, the series resistance of the solar cell reduces significantly to 0.14 Ω cm 2 and a CZTSe solar cell with efficiency of 7.2% is fabricated.

Metabolomics by Gas Chromatography-Mass Spectrometry: the combination of targeted and untargeted profiling

PubMed Central

Fiehn, Oliver

2016-01-01

Gas chromatography-mass spectrometry (GC-MS)-based metabolomics is ideal for identifying and quantitating small molecular metabolites (<650 daltons), including small acids, alcohols, hydroxyl acids, amino acids, sugars, fatty acids, sterols, catecholamines, drugs, and toxins, often using chemical derivatization to make these compounds volatile enough for gas chromatography. This unit shows that on GC-MS- based metabolomics easily allows integrating targeted assays for absolute quantification of specific metabolites with untargeted metabolomics to discover novel compounds. Complemented by database annotations using large spectral libraries and validated, standardized standard operating procedures, GC-MS can identify and semi-quantify over 200 compounds per study in human body fluids (e.g., plasma, urine or stool) samples. Deconvolution software enables detection of more than 300 additional unidentified signals that can be annotated through accurate mass instruments with appropriate data processing workflows, similar to liquid chromatography-MS untargeted profiling (LC-MS). Hence, GC-MS is a mature technology that not only uses classic detectors (‘quadrupole’) but also target mass spectrometers (‘triple quadrupole’) and accurate mass instruments (‘quadrupole-time of flight’). This unit covers the following aspects of GC-MS-based metabolomics: (i) sample preparation from mammalian samples, (ii) acquisition of data, (iii) quality control, and (iv) data processing. PMID:27038389

A thin-layer liquid culture technique for the growth of Helicobacter pylori.

PubMed

Joo, Jung-Soo; Park, Kyung-Chul; Song, Jae-Young; Kim, Dong-Hyun; Lee, Kyung-Ja; Kwon, Young-Cheol; Kim, Jung-Min; Kim, Kyung-Mi; Youn, Hee-Shang; Kang, Hyung-Lyun; Baik, Seung-Chul; Lee, Woo-Kon; Cho, Myung-Je; Rhee, Kwang-Ho

2010-08-01

Several attempts have been successful in liquid cultivation of Helicobaccter pylori. However, there is a need to improve the growth of H. pylori in liquid media in order to get affluent growth and a simple approach for examining bacterial properties. We introduce here a thin-layer liquid culture technique for the growth of H. pylori. A thin-layer liquid culture system was established by adding liquid media to a 90-mm diameter Petri dish. Optimal conditions for bacterial growth were investigated and then viability, growth curve, and released proteins were examined. Maximal growth of H. pylori was obtained by adding 3 mL of brucella broth supplemented with 10% horse to a Petri dish. H. pylori grew in both DMEM and RPMI-1640 supplemented with 10% fetal bovine serum and 0.5% yeast extract. Serum-free RPMI-1640 supported the growth of H. pylori when supplemented with dimethyl-beta-cyclodextrin (200 microg/mL) and 1% yeast extract. Under optimal growth, H. pylori grew exponentially for 28 hours, reaching a density of 3.4 OD(600) with a generation time of 3.3 hours. After 24 hours, cultures at a cell density of 1.0 OD(600) contained 1.3 +/- 0.1 x 10(9 )CFU/mL. gamma-Glutamyl transpeptidase, nuclease, superoxide dismutase, and urease were not detected in culture supernatants at 24 hours in thin-layer liquid culture, but were present at 48 hours, whereas alcohol dehydrogenase, alkylhydroperoxide reductase, catalase, and vacuolating cytotoxin were detected at 24 hours. Thin-layer liquid culture technique is feasible, and can serve as a versatile liquid culture technique for investigating bacterial properties of H. pylori.

Diagnosis of gastroenterological diseases by metabolome analysis using gas chromatography-mass spectrometry.

PubMed

Yoshida, Masaru; Hatano, Naoya; Nishiumi, Shin; Irino, Yasuhiro; Izumi, Yoshihiro; Takenawa, Tadaomi; Azuma, Takeshi

2012-01-01

Recently, metabolome analysis has been increasingly applied to biomarker detection and disease diagnosis in medical studies. Metabolome analysis is a strategy for studying the characteristics and interactions of low molecular weight metabolites under a specific set of conditions and is performed using mass spectrometry and nuclear magnetic resonance spectroscopy. There is a strong possibility that changes in metabolite levels reflect the functional status of a cell because alterations in their levels occur downstream of DNA, RNA, and protein. Therefore, the metabolite profile of a cell is more likely to represent the current status of a cell than DNA, RNA, or protein. Thus, owing to the rapid development of mass spectrometry analytical techniques metabolome analysis is becoming an important experimental method in life sciences including the medical field. Here, we describe metabolome analysis using liquid chromatography-mass spectrometry, gas chromatography-mass spectrometry (GC-MS), capillary electrophoresis-mass spectrometry, and matrix assisted laser desorption ionization-mass spectrometry. Then, the findings of studies about GC-MS-based metabolome analysis of gastroenterological diseases are summarized, and our research results are also introduced. Finally, we discuss the realization of disease diagnosis by metabolome analysis. The development of metabolome analysis using mass spectrometry will aid the discovery of novel biomarkers, hopefully leading to the early detection of various diseases.

Toward rapid analysis, forecast and discovery of bioactive compounds from herbs by jointly using thin layer chromatography and ratiometric surface-enhanced Raman spectroscopy technique.

PubMed

Gu, Xiaoling; Jin, Yang; Dong, Fang; Cai, Yueqing; You, Zhengyi; You, Junhui; Zhang, Liying; Du, Shuhu

2018-05-10

Conventional isolation and identification of active compounds from herbs have been extensively reported by using various chromatographic and spectroscopic techniques. However, how to quickly discover new bioactive ingredients from natural sources still remains a challenging task due to the interference of their similar structures or matrices. Here, we present a grand approach for rapid analysis, forecast and discovery of bioactive compounds from herbs based on a hyphenated strategy of thin layer chromatography and ratiometric surface-enhanced Raman spectroscopy. The performance of the hyphenated strategy is first evaluated by analyzing four protoberberine alkaloids, berberine (BER), coptisine (COP), palmatine (PAT) and jatrorrhizine (JAT), from a typical herb Coptidis Rhizoma as an example. It has been demonstrated that this coupling method can identify the four compounds by characteristic peaks at 728, 708, 736 and 732 cm -1 , and especially discriminate BER and COP (with similar migration distances) by ratiometric Raman intensity (I 708 /I 728 ). The corresponding limits of detection are 0.1, 0.05, 0.1 and 0.5 μM, respectively, which are about 1-2 orders of magnitude lower than those of direct observation method under 254 nm UV lamp. Based on these findings, the proposed method further guides forecast and discovery of unknown compounds from traditional Chinese herb Typhonii Rhizoma. Results infer that two trace alkaloids (BER and COP) from the n-butanol extract of Typhonii Rhizoma are found for the first time. Moreover, in vitro experiments manifest that BER can effectively decrease the viability of human glioma U87 cells by inducing cell cycle arrest in a concentration-dependent manner. Copyright © 2018 Elsevier B.V. All rights reserved.

Pyrolysis-high resolution gas chromatography and pyrolysis gas chromatography-mass spectrometry of kerogens and kerogen precursors

NASA Technical Reports Server (NTRS)

Van De Meent, D.; Brown, S. C.; Philp, R. P.; Simoneit, B. R. T.

1980-01-01

A series of kerogens and kerogen precursors isolated from DSDP samples, oil shales and recent algal mats have been examined by Curie point pyrolysis-high resolution gas chromatography and gas chromatography-mass spectrometry. This study has shown that the three main types of kerogens (marine, terrestrial and mixtures of both) can be characterized using these techniques. The marine (algal) kerogens yield principally aliphatic products and the terrestrial kerogens yield more aromatic and phenolic products with some n-alkanes and n-alkenes. The yields of n-alkanes and n-alkenes increase and phenols decrease with increasing geologic age, however, pyrolysis-GC cannot be used to characterize the influence of short term diagenesis on the kerogen structure.

Integration of electrochemistry with ultra-performance liquid chromatography/mass spectrometry.

PubMed

Cai, Yi; Zheng, Qiuling; Liu, Yong; Helmy, Roy; Loo, Joseph A; Chen, Hao

2015-01-01

This study presents the development of ultra-performance liquid chromatography (UPLC) mass spectrometry (MS) combined with electrochemistry (EC) for the first time and its application for the structural analysis of proteins/peptides that contain disulfide bonds. In our approach, a protein/peptide mixture sample undergoes a fast UPLC separation and subsequent electrochemical reduction in an electrochemical flow cell followed by online MS and tandem mass spectrometry (MS/MS) analyses. The electrochemical cell is coupled to the mass spectrometer using our recently developed desorption electrospray ionization (DESI) interface. Using this UPLC/EC/DESI-MS method, peptides that contain disulfide bonds can be differentiated from those without disulfide bonds, as the former are electroactive and reducible. MS/MS analysis of the disulfide-reduced peptide ions provides increased information on the sequence and disulfide-linkage pattern. In a reactive DESI- MS detection experiment in which a supercharging reagent was used to dope the DESI spray solvent, increased charging was obtained for the UPLC-separated proteins. Strikingly, upon online electrolytic reduction, supercharged proteins (e.g., α-lactalbumin) showed even higher charging, which will be useful in top- down protein structure MS analysis as increased charges are known to promote protein ion dissociation. Also, the separation speed and sensitivity are enhanced by approximately 1(~)2 orders of magnitude by using UPLC for the liquid chromatography (LC)/EC/MS platform, in comparison to the previously used high- performance liquid chromatography (HPLC). This UPLC/EC/DESI-MS method combines the power of fast UPLC separation, fast electrochemical conversion, and online MS structural analysis for a potentially valuable tool for proteomics research and bioanalysis.

Identification and Quantification of Pesticides in Environmental Waters With Solid Phase Microextraction and Analysis Using Field-Portable Gas Chromatography-Mass Spectrometry

DTIC Science & Technology

2004-06-10

Microextraction and Analysis using Field-Portable Gas Chromatography-Mass Spectrometry Name of Candidate: CPT Michael J. Nack...and Analysis using Field-Portable Gas Chromatography-Mass Spectrometry Beyond brief excerpts is with the permission of the copyright owner, and...Pesticides in Environmental Waters with Solid Phase Microextraction and Analysis using Field-Portable Gas Chromatography-Mass Spectrometry

Thin and thick layers of resin-based sealer cement bonded to root dentine compared: Adhesive behaviour.

PubMed

Pane, Epita S; Palamara, Joseph E A; Messer, Harold H

2015-12-01

This study aims to evaluate tensile and shear bond strengths of one epoxy (AH) and two methacrylate resin-based sealers (EZ and RS) in thin and thick layers bonded to root dentine. An alignment device was prepared for accurate positioning of 20 root dentine cylinders in a predefined gap of 0.1 or 1 mm. Sealer was placed in the interface. Bond strength tests were conducted. Mode of failures and representative surfaces were evaluated. Data were analysed using anova and post-hoc tests, with P < 0.05. The thick layer of sealer produced higher bond strength, except for the shear bond strength of EZ. Significant differences between thin and thick layers were found only in tensile bond strengths of AH and RS. Mixed type of failure was constantly found with all sealers. Bond strengths of thick layers of resin-based sealers to root dentine tended to be higher than with thin layers. © 2015 Australian Society of Endodontology.

Multi-Instrument Characterization of the Surfaces and Materials in Microfabricated, Carbon Nanotube-Templated Thin Layer Chromatography Plates. An Analogy to ‘The Blind Men and the Elephant’

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

Jensen, David S.; Kanyal, Supriya S.; Madaan, Nitesh

Herein we apply a suite of surface/materials analytical tools to characterize some of the materials created in the production of microfabricated thin layer chromatography plates. Techniques used include X-ray photoelectron spectroscopy (XPS), valence band spectroscopy, static time-of-flight secondary ion spectrometry (ToF-SIMS) in both positive and negative ion modes, Rutherford backscattering spectroscopy (RBS), and helium ion microscopy (HIM). Materials characterized include: the Si(100) substrate with native oxide: Si/SiO2, alumina (35 nm) deposited as a diffusion barrier on the Si/SiO2: Si/SiO2/Al2O3, iron (6 nm) thermally evaporated on the Al2O3: Si/SiO2/Al2O3/Fe, the iron film annealed in H2 to make Fe catalyst nanoparticles: Si/SiO2/Al2O3/Fe(NP),more » and carbon nanotubes (CNTs) grown from the Fe nanoparticles: Si/SiO2/Al2O3/Fe(NP)/CNT. The Fe thin films and nanoparticles are found in an oxidized state. Some of the analyses of the CNTs/CNT forests reported appear to be unique: the CNT forest appears to exhibit an interesting ‘channeling’ phenomenon by RBS, we observe an odd-even effect in the ToF-SIMS spectra of Cn- species for n = 1 – 6, with ions at even n showing greater intensity than the neighboring signals, and ions with n ≥ 6 showing a steady decrease in intensity, and valence band characterization of CNTs using X-radiation is reported. The information obtained from the combination of the different analytical tools provides a more complete understanding of our materials than a single technique, which is analogous to the story of ‘The Blind Men and the Elephant’. (Of course there is increasing emphasis on the use of multiple characterization tools in surface and materials analysis.) The raw XPS and ToF-SIMS spectra from this study will be submitted to Surface Science Spectra for archiving.« less

Liquid chromatography fractionation with gas chromatography/mass spectrometry and preparative gas chromatography-nuclear magnetic resonance analysis of selected nonylphenol polyethoxylates.

PubMed

Wu, Ze-ying; Rühle, Christian P G; Marriott, Philip J

2011-07-01

Commercial nonylphenol polyethoxylates, designated as NPnEOs, where n is the number of ethoxy groups, comprise a range of ethoxylate groups. According to the starting material nonylphenol, they may also be composed of a complex mix of isomeric nonyl substituents. In order to study more fully the heterogeneity arising from both the ethoxylate and nonyl groups, a mixture of NPnEOs is first fractionated by normal phase liquid chromatography (NPLC) into separate fractions comprising individual ethoxymers, n. Preparative collection of each early elution ethoxymer fraction allows further separation of different isomeric nonyl group components by using analytical gas chromatography/mass spectrometry (GC/MS). The nonyl isomers are not resolved in the NPLC method. The distribution of the isomeric nonyl side chain of different ethoxymers bears close resemblance with each other, and also with the original nonylphenol starting material, although separation efficiency of the nonyl isomers for each ethoxymer decreases with increasing ethoxymer number. Mass spectrometry of the separated isomers display close similarity for presumed equivalent isomers in each fraction, based on elution order of the nonyl isomers. This suggests that each corresponding peak has the same isomer structure. Mass spectra are interpreted based on branching within the nonyl side chain. Preparative GC coupled with MS and nuclear magnetic resonance spectroscopy elucidated the molecular structure of one of the resolved isomers as 4-(1,3-dimethyl-1-propyl-butyl)-phenol diethoxylate. Copyright © 2011 Elsevier B.V. All rights reserved.

[Confirming Indicators of Qualitative Results by Chromatography-mass Spectrometry in Biological Samples].

PubMed

Liu, S D; Zhang, D M; Zhang, W; Zhang, W F

2017-04-01

Because of the exist of complex matrix, the confirming indicators of qualitative results for toxic substances in biological samples by chromatography-mass spectrometry are different from that in non-biological samples. Even in biological samples, the confirming indicators are different in various application areas. This paper reviews the similarities and differences of confirming indicators for the analyte in biological samples by chromatography-mass spectrometry in the field of forensic toxicological analysis and other application areas. These confirming indicators include retention time （RT）, relative retention time （RRT）, signal to noise （S/N）, characteristic ions, relative abundance of characteristic ions, parent ion-daughter ion pair and abundance ratio of ion pair, etc. Copyright© by the Editorial Department of Journal of Forensic Medicine.

Conversion treatment of thin titanium layer deposited on carbon steel

NASA Astrophysics Data System (ADS)

Benarioua, Younes; Wendler, Bogdan; Chicot, Didier

2018-05-01

The present study has been conducted in order to obtain titanium carbide layer using a conversion treatment consisting of two main steps. In the first step a thin pure titanium layer was deposited on 120C4 carbon steel by PVD. In the second step, the carbon atoms from the substrate diffuse to the titanium coating due to a vacuum annealing treatment and the Ti coating transforms into titanium carbide. Depending on the annealing temperature a partial or complete conversion into TiC is obtained. The hardness of the layer can be expected to differ depending on the processing temperatures. By a systematic study of the hardness as a function of the applied load, we confirm the process of growth of the layer.

High-performance a-IGZO thin-film transistor with conductive indium-tin-oxide buried layer

NASA Astrophysics Data System (ADS)

Ahn, Min-Ju; Cho, Won-Ju

2017-10-01

In this study, we fabricated top-contact top-gate (TCTG) structure of amorphous indium-gallium-zinc oxide (a-IGZO) thin-film transistors (TFTs) with a thin buried conductive indium-tin oxide (ITO) layer. The electrical performance of a-IGZO TFTs was improved by inserting an ITO buried layer under the IGZO channel. Also, the effect of the buried layer's length on the electrical characteristics of a-IGZO TFTs was investigated. The electrical performance of the transistors improved with increasing the buried layer's length: a large on/off current ratio of 1.1×107, a high field-effect mobility of 35.6 cm2/Vs, a small subthreshold slope of 116.1 mV/dec, and a low interface trap density of 4.2×1011 cm-2eV-1 were obtained. The buried layer a-IGZO TFTs exhibited enhanced transistor performance and excellent stability against the gate bias stress.

Stepwise crystallization and the layered distribution in crystallization kinetics of ultra-thin poly(ethylene terephthalate) film

NASA Astrophysics Data System (ADS)

Zuo, Biao; Xu, Jianquan; Sun, Shuzheng; Liu, Yue; Yang, Juping; Zhang, Li; Wang, Xinping

2016-06-01

Crystallization is an important property of polymeric materials. In conventional viewpoint, the transformation of disordered chains into crystals is usually a spatially homogeneous process (i.e., it occurs simultaneously throughout the sample), that is, the crystallization rate at each local position within the sample is almost the same. Here, we show that crystallization of ultra-thin poly(ethylene terephthalate) (PET) films can occur in the heterogeneous way, exhibiting a stepwise crystallization process. We found that the layered distribution of glass transition dynamics of thin film modifies the corresponding crystallization behavior, giving rise to the layered distribution of the crystallization kinetics of PET films, with an 11-nm-thick surface layer having faster crystallization rate and the underlying layer showing bulk-like behavior. The layered distribution in crystallization kinetics results in a particular stepwise crystallization behavior during heating the sample, with the two cold-crystallization temperatures separated by up to 20 K. Meanwhile, interfacial interaction is crucial for the occurrence of the heterogeneous crystallization, as the thin film crystallizes simultaneously if the interfacial interaction is relatively strong. We anticipate that this mechanism of stepwise crystallization of thin polymeric films will allow new insight into the chain organization in confined environments and permit independent manipulation of localized properties of nanomaterials.

Stepwise crystallization and the layered distribution in crystallization kinetics of ultra-thin poly(ethylene terephthalate) film

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

Zuo, Biao, E-mail: chemizuo@zstu.edu.cn, E-mail: wxinping@yahoo.com; Xu, Jianquan; Sun, Shuzheng

2016-06-21

Crystallization is an important property of polymeric materials. In conventional viewpoint, the transformation of disordered chains into crystals is usually a spatially homogeneous process (i.e., it occurs simultaneously throughout the sample), that is, the crystallization rate at each local position within the sample is almost the same. Here, we show that crystallization of ultra-thin poly(ethylene terephthalate) (PET) films can occur in the heterogeneous way, exhibiting a stepwise crystallization process. We found that the layered distribution of glass transition dynamics of thin film modifies the corresponding crystallization behavior, giving rise to the layered distribution of the crystallization kinetics of PET films,more » with an 11-nm-thick surface layer having faster crystallization rate and the underlying layer showing bulk-like behavior. The layered distribution in crystallization kinetics results in a particular stepwise crystallization behavior during heating the sample, with the two cold-crystallization temperatures separated by up to 20 K. Meanwhile, interfacial interaction is crucial for the occurrence of the heterogeneous crystallization, as the thin film crystallizes simultaneously if the interfacial interaction is relatively strong. We anticipate that this mechanism of stepwise crystallization of thin polymeric films will allow new insight into the chain organization in confined environments and permit independent manipulation of localized properties of nanomaterials.« less

Epitaxially influenced boundary layer model for size effect in thin metallic films

NASA Astrophysics Data System (ADS)

Bažant, Zdeněk P.; Guo, Zaoyang; Espinosa, Horacio D.; Zhu, Yong; Peng, Bei

2005-04-01

It is shown that the size effect recently observed by Espinosa et al., [J. Mech. Phys. Solids51, 47 (2003)] in pure tension tests on free thin metallic films can be explained by the existence of a boundary layer of fixed thickness, located at the surface of the film that was attached onto the substrate during deposition. The boundary layer is influenced by the epitaxial effects of crystal growth on the dislocation density and texture (manifested by prevalent crystal plane orientations). This influence is assumed to cause significantly elevated yield strength. Furthermore, the observed gradual postpeak softening, along with its size independence, which is observed in short film strips subjected to pure tension, is explained by slip localization, originating at notch-like defects, and by damage, which can propagate in a stable manner when the film strip under pure tension is sufficiently thin and short. For general applications, the present epitaxially influenced boundary layer model may be combined with the classical strain-gradient plasticity proposed by Gao et al., [J. Mech. Phys. Solids 47, 1239 (1999)], and it is shown that this combination is necessary to fit the test data on both pure tension and bending of thin films by one and the same theory. To deal with films having different crystal grain sizes, the Hall-Petch relation for the yield strength dependence on the grain size needs to be incorporated into the combined theory. For very thin films, in which a flattened grain fills the whole film thickness, the Hall-Petch relation needs a cutoff, and the asymptotic increase of yield strength with diminishing film thickness is then described by the extension of Nix's model of misfit dislocations by Zhang and Zhou [J. Adv. Mater. 38, 51 (2002)]. The final result is a proposal of a general theory for strength, size effect, hardening, and softening of thin metallic films.

Sub-10-Minute Characterization of an Ultrahigh Molar Mass Polymer by Multi-detector Hydrodynamic Chromatography

USDA-ARS?s Scientific Manuscript database

Molar mass averages, distributions, and architectural information of polymers are routinely obtained using size-exclusion chromatography (SEC). It has previously been shown that ultrahigh molar mass polymers may experience degradation during SEC analysis, leading to inaccurate molar mass averages a...

Quantification of 11-Carboxy-Delta-9-Tetrahydrocannabinol (THC-COOH) in Meconium Using Gas Chromatography/Mass Spectrometry (GC/MS).

PubMed

Peat, Judy; Davis, Brehon; Frazee, Clint; Garg, Uttam

2016-01-01

Maternal substance abuse is an ongoing concern and detecting drug use during pregnancy is an important component of neonatal care when drug abuse is suspected. Meconium is the preferred specimen for drug testing because it is easier to collect than neonatal urine and it provides a much broader time frame of drug exposure. We describe a method for quantifying 11-carboxy-delta-9-tetrahydrocannabinol (THC-COOH) in meconium. After adding a labeled internal standard (THC-COOH D9) and acetonitrile, samples are sonicated to release both free and conjugated THC-COOH. The acetonitrile/aqueous layer is removed and mixed with a strong base to hydrolyze the conjugated THC-COOH. The samples are then extracted with an organic solvent mixture as part of a sample "cleanup." The organic solvent layer is discarded and the remaining aqueous sample is acidified. Following extraction with a second organic mixture, the organic layer is removed and concentrated to dryness. The resulting residue is converted to a trimethylsilyl (TMS) derivative and analyzed using gas chromatography/mass spectrometry (GC/MS) in selective ion monitoring (SIM) mode.

Correlation between active layer thickness and ambient gas stability in IGZO thin-film transistors

NASA Astrophysics Data System (ADS)

Gao, Xu; Lin, Meng-Fang; Mao, Bao-Hua; Shimizu, Maki; Mitoma, Nobuhiko; Kizu, Takio; Ou-Yang, Wei; Nabatame, Toshihide; Liu, Zhi; Tsukagoshi, Kazuhito; Wang, Sui-Dong

2017-01-01

Decreasing the active layer thickness has been recently reported as an alternative way to achieve fully depleted oxide thin-film transistors for the realization of low-voltage operations. However, the correlation between the active layer thickness and device resistivity to environmental changes is still unclear, which is important for the optimized design of oxide thin-film transistors. In this work, the ambient gas stability of IGZO thin-film transistors is found to be strongly correlated to the IGZO thickness. The TFT with the thinnest IGZO layer shows the highest intrinsic electron mobility in a vacuum, which is greatly reduced after exposure to O2/air. The device with a thick IGZO layer shows similar electron mobility in O2/air, whereas the mobility variation measured in the vacuum is absent. The thickness dependent ambient gas stability is attributed to a high-mobility region in the IGZO surface vicinity with less sputtering-induced damage, which will become electron depleted in O2/air due to the electron transfer to adsorbed gas molecules. The O2 adsorption and deduced IGZO surface band bending is demonstrated by the ambient-pressure x-ray photoemission spectroscopy results.

Recent Advances in Gas Barrier Thin Films via Layer-by-Layer Assembly of Polymers and Platelets.

PubMed

Priolo, Morgan A; Holder, Kevin M; Guin, Tyler; Grunlan, Jaime C

2015-05-01

Layer-by-layer (LbL) assembly has emerged as the leading non-vacuum technology for the fabrication of transparent, super gas barrier films. The super gas barrier performance of LbL deposited films has been demonstrated in numerous studies, with a variety of polyelectrolytes, to rival that of metal and metal oxide-based barrier films. This Feature Article is a mini-review of LbL-based multilayer thin films with a 'nanobrick wall' microstructure comprising polymeric mortar and nano-platelet bricks that impart high gas barrier to otherwise permeable polymer substrates. These transparent, water-based thin films exhibit oxygen transmission rates below 5 × 10(-3) cm(3) m(-2) day(-1) atm(-1) and lower permeability than any other barrier material reported. In an effort to put this technology in the proper context, incumbent technologies such as metallized plastics, metal oxides, and flake-filled polymers are briefly reviewed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Mass-physical properties of surficial sediments on the Rhoˆne continental margin: implications for the nepheloid benthic layer

NASA Astrophysics Data System (ADS)

Chassefiere, Bernard

1990-09-01

Mass-physical properties of the surficial (upper 5 m) sediments on the Gulf of Lions continental margin were analysed, from more than 100 short (1 m) and longer (5 m) cores obtained during several cruises. Data include water content, unit weight, Atterberg limits (liquid limit, plastic limit, plasticity index), shear strength and compression index, and are used to determine: first, the mass property distribution, according to the main parameters influencing mass-physical properties; the relationships between these properties and the nepheloid layer on the shelf. The shoreline (lagoons) and inner shelf are characterized by low density and shear strength and high water content deposits, due to electrochemical flocculation of the sediment. The outer shelf is blanketed by higher density and shear strength and lower water content deposits generated by normal settling of suspended particles. On the inner shelf, during river peak discharges, a short-term thin bottom layer of "yogurt-like" [ FASS (1985) Geomarine Letters, 4, 147-152; FASS (1986) Continental Shelf Research, 6, 189-208] fluid-mud (unit weight lower than 1.3 mg m -3) is supplied, by a bottom nepheloid layer. During stormy periods, this "yogurt-like" layer (about 10 cm thick) partly disappears by resuspension of suspended particulate matter; this is advected, in the bottom nepheloid layer, over the shelf and the canyons within the upper slope.

Separation of paralytic shellfish poisoning toxins on Chromarods-SIII by thin-layer chromatography with the Iatroscan (mark 5) and flame thermionic detection.

PubMed

Indrasena, W M; Ackman, R G; Gill, T A

1999-09-10

Thin-layer chromatography (TLC) on Chromarods-SIII with the Iatroscan (Mark-5) and a flame thermionic detector (FTID) was used to develop a rapid method for the detection of paralytic shellfish poisoning (PSP) toxins. The effect of variation in hydrogen (H2) flow, air flow, scan time and detector current on the FTID peak response for both phosphatidylcholine (PC) and PSP were studied in order to define optimum detection conditions. A combination of hydrogen and air flow-rates of 50 ml/min and 1.5-2.0 l/min respectively, along with a scan time of 40 s/rod and detector current of 3.0 A (ampere) or above were found to yield the best results for the detection of PSP compounds. Increasing the detector current level to as high as 3.3 A gave about 130 times more FTID response than did flame ionization detection (FID), for PSP components. Quantities of standards as small as 1 ng neosaxitoxin (NEO), 5 ng saxitoxin (STX), 5 ng B1-toxins (B1), 2 ng gonyautoxin (GTX) 2/3, 6 ng GTX 1/4 and 6 ng C-toxins (C1/C2) could be detected with the FTID. The method detection limits for toxic shellfish tissues using the FTID were 0.4, 2.1, 0.8 and 2.5 micrograms per g tissue for GTX 2/3, STX, NEO and C toxins, respectively. The FTID response increased with increasing detector current and with increasing the scan time. Increasing hydrogen and air flow-rates resulted in decreasing sensitivity within defined limits. Numerous solvent systems were tested, and, solvent consisting of chloroform: methanol-water-acetic acid (30:50:8:2) could separate C toxins from GTX, which eluted ahead of NEO and STX. Accordingly, TLC/FTID with the Iatroscan (Mark-5) seems to be a promising, relatively inexpensive and rapid method of screening plant and animal tissues for PSP toxins.

Separation and purification of astaxanthin from Phaffia rhodozyma by preparative high-speed counter-current chromatography.

PubMed

Du, Xiping; Dong, Congcong; Wang, Kai; Jiang, Zedong; Chen, Yanhong; Yang, Yuanfan; Chen, Feng; Ni, Hui

2016-09-01

An effective high-speed counter-current chromatography (HSCCC) method was established for the preparative isolation and purification of astaxanthin from Phaffia rhodozyma. With a two-phase solvent system composed of n-hexane-acetone-ethanol-water (1:1:1:1, v/v/v/v), 100mg crude extract of P. rhodozyma was separated to yield 20.6mg of astaxanthin at 92.0% purity. By further one step silica gel column chromatography, the purity reached 99.0%. The chemical structure of astaxanthin was confirmed by thin layer chromatography (TLC), UV spectroscopy scanning, high performance liquid chromatography with a ZORBAX SB-C18 column and a Waters Nova-pak C18 column, and ESI/MS/MS. Copyright © 2016 Elsevier B.V. All rights reserved.

Enhanced stability of thin film transistors with double-stacked amorphous IWO/IWO:N channel layer

NASA Astrophysics Data System (ADS)

Lin, Dong; Pi, Shubin; Yang, Jianwen; Tiwari, Nidhi; Ren, Jinhua; Zhang, Qun; Liu, Po-Tsun; Shieh, Han-Ping

2018-06-01

In this work, bottom-gate top-contact thin film transistors with double-stacked amorphous IWO/IWO:N channel layer were fabricated. Herein, amorphous IWO and N-doped IWO were deposited as front and back channel layers, respectively, by radio-frequency magnetron sputtering. The electrical characteristics of the bi-layer-channel thin film transistors (TFTs) were examined and compared with those of single-layer-channel (i.e., amorphous IWO or IWO:N) TFTs. It was demonstrated to exhibit a high mobility of 27.2 cm2 V‑1 s‑1 and an on/off current ratio of 107. Compared to the single peers, bi-layer a-IWO/IWO:N TFTs showed smaller hysteresis and higher stability under negative bias stress and negative bias temperature stress. The enhanced performance could be attributed to its unique double-stacked channel configuration, which successfully combined the merits of the TFTs with IWO and IWO:N channels. The underlying IWO thin film provided percolation paths for electron transport, meanwhile, the top IWO:N layer reduced the bulk trap densities. In addition, the IWO channel/gate insulator interface had reduced defects, and IWO:N back channel surface was insensitive to the ambient atmosphere. Overall, the proposed bi-layer a-IWO/IWO:N TFTs show potential for practical applications due to its possibly long-term serviceability.

Treatment of ice cover and other thin elastic layers with the parabolic equation method.

PubMed

Collins, Michael D

2015-03-01

The parabolic equation method is extended to handle problems involving ice cover and other thin elastic layers. Parabolic equation solutions are based on rational approximations that are designed using accuracy constraints to ensure that the propagating modes are handled properly and stability constrains to ensure that the non-propagating modes are annihilated. The non-propagating modes are especially problematic for problems involving thin elastic layers. It is demonstrated that stable results may be obtained for such problems by using rotated rational approximations [Milinazzo, Zala, and Brooke, J. Acoust. Soc. Am. 101, 760-766 (1997)] and generalizations of these approximations. The approach is applied to problems involving ice cover with variable thickness and sediment layers that taper to zero thickness.

Derivatization reagents in liquid chromatography/electrospray ionization tandem mass spectrometry.

PubMed

Santa, Tomofumi

2011-01-01

Liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) is one of the most prominent analytical techniques owing to its inherent selectivity and sensitivity. In LC/ESI-MS/MS, chemical derivatization is often used to enhance the detection sensitivity. Derivatization improves the chromatographic separation, and enhances the mass spectrometric ionization efficiency and MS/MS detectability. In this review, an overview of the derivatization reagents which have been applied to LC/ESI-MS/MS is presented, focusing on the applications to low molecular weight compounds. 2010 John Wiley & Sons, Ltd.

Review of Peak Detection Algorithms in Liquid-Chromatography-Mass Spectrometry

PubMed Central

Zhang, Jianqiu; Gonzalez, Elias; Hestilow, Travis; Haskins, William; Huang, Yufei

2009-01-01

In this review, we will discuss peak detection in Liquid-Chromatography-Mass Spectrometry (LC/MS) from a signal processing perspective. A brief introduction to LC/MS is followed by a description of the major processing steps in LC/MS. Specifically, the problem of peak detection is formulated and various peak detection algorithms are described and compared. PMID:20190954

A thin layer electrochemical cell for disinfection of water contaminated with Staphylococcus aureus

PubMed Central

Gusmão, Isabel C. P.; Moraes, Peterson B.; Bidoia, Ederio D.

2009-01-01

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 chloride-free 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. PMID:24031410

Validation of lipolysis product extraction from aqueous/biological samples, separation and quantification by thin-layer chromatography with flame ionization detection analysis using O-cholesteryl ethylene glycol as a new internal standard.

PubMed

Cavalier, Jean-François; Lafont, Dominique; Boullanger, Paul; Houisse, David; Giallo, Jacqueline; Ballester, Jean-Michel; Carrière, Frédéric

2009-09-11

A general and easily accessible method for the extraction followed by the simultaneous separation and quantitative determination of triacylglycerols, diacylglycerols, monoacylglycerols and free fatty acids has been improved and optimized based on existing protocols using liquid-phase extraction and thin-layer chromatography coupled to flame ionization detection (TLC/FID Iatroscan). After lipid extraction in the presence of a suitable new synthetic internal standard, namely CholE1, a single elution step using n-heptane/diethyl ether/formic acid (55:45:1, v/v/v) was applied. This method was validated in line with international bioanalytical method validation guidelines using two different matrix systems: purified water and human gastro-intestinal fluid. Overall, the assay was found to have high levels of precision with coefficients of variation ranging from 1.48% to 11.0% and accuracy ranging from -13.3% to +5.79% RE. The confidence limits of the lipid mean recovery rates varied between 89.9% and 104%. This method is therefore highly suitable for quantifying the lipolysis products generated in vitro during the hydrolysis of various fats and oils by digestive lipases, as well as those collected from the gastro-intestinal tract in the course of human clinical studies on lipid digestion.

Multi-layer thin-film electrolytes for metal supported solid oxide fuel cells

NASA Astrophysics Data System (ADS)

Haydn, Markus; Ortner, Kai; Franco, Thomas; Uhlenbruck, Sven; Menzler, Norbert H.; Stöver, Detlev; Bräuer, Günter; Venskutonis, Andreas; Sigl, Lorenz S.; Buchkremer, Hans-Peter; Vaßen, Robert

2014-06-01

A key to the development of metal-supported solid oxide fuel cells (MSCs) is the manufacturing of gas-tight thin-film electrolytes, which separate the cathode from the anode. This paper focuses the electrolyte manufacturing on the basis of 8YSZ (8 mol.-% Y2O3 stabilized ZrO2). The electrolyte layers are applied by a physical vapor deposition (PVD) gas flow sputtering (GFS) process. The gas-tightness of the electrolyte is significantly improved when sequential oxidic and metallic thin-film multi-layers are deposited, which interrupt the columnar grain structure of single-layer electrolytes. Such electrolytes with two or eight oxide/metal layers and a total thickness of about 4 μm obtain leakage rates of less than 3 × 10-4 hPa dm3 s-1 cm-2 (Δp: 100 hPa) at room temperature and therefore fulfill the gas tightness requirements. They are also highly tolerant with respect to surface flaws and particulate impurities which can be present on the graded anode underground. MSC cell tests with double-layer and multilayer electrolytes feature high power densities more than 1.4 W cm-2 at 850 °C and underline the high potential of MSC cells.

Characterization of goat colostrum oligosaccharides by nano-liquid chromatography on chip quadrupole time-of-flight mass spectrometry and hydrophilic interaction liquid chromatography-quadrupole mass spectrometry

PubMed Central

Martín-Ortiz, A.; Salcedo, J.; Barile, D.; Bunyatratchata, A.; Moreno, F.J.; Martin-García, I.; Clemente, A.; Sanz, M.L.; Ruiz-Matute, A.I.

2016-01-01

A detailed qualitative and quantitative characterization of goat colostrum oligosaccharides (GCO) has been carried out for the first time. Defatted and deproteinized colostrum samples, previously treated by size exclusion chromatography (SEC) to remove lactose, were analyzed by nanoflow liquid chromatography-quadrupole-time of flight mass spectrometry (Nano-LC-Chip-Q-TOF MS). Up to 78 oligosaccharides containing hexose, hexosamine, fucose, N-acetylneuraminic acid or N-glycolylneuraminic acid monomeric units were identified in the samples, some of them detected for the first time in goat colostra. As a second step, a hydrophilic interaction liquid chromatography coupled to mass spectrometry (HILIC-MS) methodology was developed for the separation and quantitation of the main GCO, both acidic and neutral carbohydrates. Among other experimental chromatographic conditions, mobile phase additives and column temperature were evaluated in terms of retention time, resolution, peak width and symmetry of target carbohydrates. Narrow peaks (wh: 0.2–0.6 min) and good symmetry (As: 0.8–1.4) were obtained for GCO using an acetonitrile:water gradient with 0.1% ammonium hydroxide at 40 °C. These conditions were selected to quantify the main oligosaccharides in goat colostrum samples. Values ranging from 140 to 315 mg L−1 for neutral oligosaccharides and from 83 to 251 mg L−1 for acidic oligosaccharides were found. The combination of both techniques resulted to be useful to achieve a comprehensive characterization of GCO. PMID:26427327

Characterization of goat colostrum oligosaccharides by nano-liquid chromatography on chip quadrupole time-of-flight mass spectrometry and hydrophilic interaction liquid chromatography-quadrupole mass spectrometry.

PubMed

Martín-Ortiz, A; Salcedo, J; Barile, D; Bunyatratchata, A; Moreno, F J; Martin-García, I; Clemente, A; Sanz, M L; Ruiz-Matute, A I

2016-01-08

A detailed qualitative and quantitative characterization of goat colostrum oligosaccharides (GCO) has been carried out for the first time. Defatted and deproteinized colostrum samples, previously treated by size exclusion chromatography (SEC) to remove lactose, were analyzed by nanoflow liquid chromatography-quadrupole-time of flight mass spectrometry (Nano-LC-Chip-Q-TOF MS). Up to 78 oligosaccharides containing hexose, hexosamine, fucose, N-acetylneuraminic acid or N-glycolylneuraminic acid monomeric units were identified in the samples, some of them detected for the first time in goat colostra. As a second step, a hydrophilic interaction liquid chromatography coupled to mass spectrometry (HILIC-MS) methodology was developed for the separation and quantitation of the main GCO, both acidic and neutral carbohydrates. Among other experimental chromatographic conditions, mobile phase additives and column temperature were evaluated in terms of retention time, resolution, peak width and symmetry of target carbohydrates. Narrow peaks (wh: 0.2-0.6min) and good symmetry (As: 0.8-1.4) were obtained for GCO using an acetonitrile:water gradient with 0.1% ammonium hydroxide at 40°C. These conditions were selected to quantify the main oligosaccharides in goat colostrum samples. Values ranging from 140 to 315mgL(-1) for neutral oligosaccharides and from 83 to 251mgL(-1) for acidic oligosaccharides were found. The combination of both techniques resulted to be useful to achieve a comprehensive characterization of GCO. Copyright © 2015 Elsevier B.V. All rights reserved.

Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates.

PubMed

Moerdijk-Poortvliet, Tanja C W; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J; Boschker, Henricus T S

2015-07-15

We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although LC/IRMS is expected to be more accurate and precise, no direct comparison has been reported. GC/IRMS with the aldonitrile penta-acetate (ANPA) derivatisation method was compared with LC/IRMS without derivatisation. A large number of glucose standards and a variety of natural samples were analysed for five neutral carbohydrates at natural abundance as well as at (13)C-enriched levels. Gas chromatography/chemical ionisation mass spectrometry (GC/CIMS) was applied to check for incomplete derivatisation of the carbohydrate, which would impair the accuracy of the GC/IRMS method. The LC/IRMS technique provided excellent precision (±0.08‰ and ±3.1‰ at natural abundance and enrichment levels, respectively) for the glucose standards and this technique proved to be superior to GC/IRMS (±0.62‰ and ±19.8‰ at natural abundance and enrichment levels, respectively). For GC/IRMS measurements the derivatisation correction and the conversion of carbohydrates into CO2 had a considerable effect on the measured δ(13)C values. However, we did not find any significant differences in the accuracy of the two techniques over the full range of natural δ(13)C abundances and (13)C-labelled glucose. The difference in the performance of GC/IRMS and LC/IRMS diminished when the δ(13)C values were measured in natural samples, because the chromatographic performance and background correction became critical factors, particularly for LC/IRMS. The derivatisation of carbohydrates for the GC/IRMS method was complete. Although both LC/IRMS and GC/IRMS are reliable techniques for compound-specific stable carbon isotope analysis of carbohydrates (provided that derivatisation is complete and the

Bias of shear wave elasticity measurements in thin layer samples and a simple correction strategy.

PubMed

Mo, Jianqiang; Xu, Hao; Qiang, Bo; Giambini, Hugo; Kinnick, Randall; An, Kai-Nan; Chen, Shigao; Luo, Zongping

2016-01-01

Shear wave elastography (SWE) is an emerging technique for measuring biological tissue stiffness. However, the application of SWE in thin layer tissues is limited by bias due to the influence of geometry on measured shear wave speed. In this study, we investigated the bias of Young's modulus measured by SWE in thin layer gelatin-agar phantoms, and compared the result with finite element method and Lamb wave model simulation. The result indicated that the Young's modulus measured by SWE decreased continuously when the sample thickness decreased, and this effect was more significant for smaller thickness. We proposed a new empirical formula which can conveniently correct the bias without the need of using complicated mathematical modeling. In summary, we confirmed the nonlinear relation between thickness and Young's modulus measured by SWE in thin layer samples, and offered a simple and practical correction strategy which is convenient for clinicians to use.

Enhanced electrical properties of oxide semiconductor thin-film transistors with high conductivity thin layer insertion for the channel region

NASA Astrophysics Data System (ADS)

Nguyen, Cam Phu Thi; Raja, Jayapal; Kim, Sunbo; Jang, Kyungsoo; Le, Anh Huy Tuan; Lee, Youn-Jung; Yi, Junsin

2017-02-01

This study examined the performance and the stability of indium tin zinc oxide (ITZO) thin film transistors (TFTs) by inserting an ultra-thin indium tin oxide (ITO) layer at the active/insulator interface. The electrical properties of the double channel device (ITO thickness of 5 nm) were improved in comparison with the single channel ITZO or ITO devices. The TFT characteristics of the device with an ITO thickness of less than 5 nm were degraded due to the formation of an island-like morphology and the carriers scattering at the active/insulator interface. The 5 nm-thick ITO inserted ITZO TFTs (optimal condition) exhibited a superior field effect mobility (∼95 cm2/V·s) compared with the ITZO-only TFTs (∼34 cm2/V·s). The best characteristics of the TFT devices with double channel layer are due to the lowest surface roughness (0.14 nm) and contact angle (50.1°) that result in the highest hydrophicility, and the most effective adhesion at the surface. Furthermore, the threshold voltage shifts for the ITO/ITZO double layer device decreased to 0.80 and -2.39 V compared with 6.10 and -6.79 V (for the ITZO only device) under positive and negative bias stress, respectively. The falling rates of EA were 0.38 eV/V and 0.54 eV/V for the ITZO and ITO/ITZO bi-layer devices, respectively. The faster falling rate of the double channel devices suggests that the trap density, including interface trap and semiconductor bulk trap, can be decreased by the ion insertion of a very thin ITO film into the ITZO/SiO2 reference device. These results demonstrate that the double active layer TFT can potentially be applied to the flat panel display.

Integrated enzyme reactor and high resolving chromatography in "sub-chip" dimensions for sensitive protein mass spectrometry.

PubMed

Hustoft, Hanne Kolsrud; Brandtzaeg, Ole Kristian; Rogeberg, Magnus; Misaghian, Dorna; Torsetnes, Silje Bøen; Greibrokk, Tyge; Reubsaet, Léon; Wilson, Steven Ray; Lundanes, Elsa

2013-12-16

Reliable, sensitive and automatable analytical methodology is of great value in e.g. cancer diagnostics. In this context, an on-line system for enzymatic cleavage of proteins, subsequent peptide separation by liquid chromatography (LC) with mass spectrometric detection has been developed using "sub-chip" columns (10-20 μm inner diameter, ID). The system could detect attomole amounts of isolated cancer biomarker progastrin-releasing peptide (ProGRP), in a more automatable fashion compared to previous methods. The workflow combines protein digestion using an 20 μm ID immobilized trypsin reactor with a polymeric layer of 2-hydroxyethyl methacrylate-vinyl azlactone (HEMA-VDM), desalting on a polystyrene-divinylbenzene (PS-DVB) monolithic trap column, and subsequent separation of resulting peptides on a 10 μm ID (PS-DVB) porous layer open tubular (PLOT) column. The high resolution of the PLOT columns was maintained in the on-line system, resulting in narrow chromatographic peaks of 3-5 seconds. The trypsin reactors provided repeatable performance and were compatible with long-term storage.

Resistivity scaling due to electron surface scattering in thin metal layers

NASA Astrophysics Data System (ADS)

Zhou, Tianji; Gall, Daniel

2018-04-01

The effect of electron surface scattering on the thickness-dependent electrical resistivity ρ of thin metal layers is investigated using nonequilibrium Green's function density functional transport simulations. Cu(001) thin films with thickness d =1 -2 nm are used as a model system, employing a random one-monolayer-high surface roughness and frozen phonons to cause surface and bulk scattering, respectively. The zero-temperature resistivity increases from 9.7 ±1.0 μ Ω cm at d =1.99 nm to 18.7 ±2.6 μ Ω cm at d =0.9 0 nm, contradicting the asymptotic T =0 prediction from the classical Fuchs-Sondheimer model. At T =9 00 K, ρ =5.8 ±0.1 μ Ω cm for bulk Cu and ρ =13.4 ±1.1 and 22.5 ±2.4 μ Ω cm for layers with d =1.99 and 0.90 nm, respectively, indicating an approximately additive phonon contribution which, however, is smaller than for bulk Cu or atomically smooth layers. The overall data indicate that the resistivity contribution from surface scattering is temperature-independent and proportional to 1 /d , suggesting that it can be described using a surface-scattering mean-free path λs for 2D transport which is channel-independent and proportional to d . Data fitting indicates λs=4 ×d for the particular simulated Cu(001) surfaces with a one-monolayer-high surface roughness. The 1 /d dependence deviates considerably from previous 1 /d2 predictions from quantum models, indicating that the small-roughness approximation in these models is not applicable to very thin (<2 nm) layers, where the surface roughness is a considerable fraction of d .

Electromagnetic shielding effectiveness of a thin silver layer deposited onto PET film via atmospheric pressure plasma reduction

NASA Astrophysics Data System (ADS)

Oh, Hyo-Jun; Dao, Van-Duong; Choi, Ho-Suk

2018-03-01

This study presents the first use of a plasma reduction reaction under atmospheric pressure to fabricate a thin silver layer on polyethylene terephthalate (PET) film without the use of toxic chemicals, high voltages, or an expensive vacuum apparatus. The developed film is applied to electromagnetic interference (EMI) shielding. After repeatedly depositing a silver layer through a plasma reduction reaction on PET, we can successfully fabricate a uniformly deposited thin silver layer. It was found that both the particle size and film thickness of thin silver layers fabricated at different AgNO3 concentrations increase with an increase in the concentration of AgNO3. However, the roughness of the thin silver layer decreases when increasing the concentration of AgNO3 from 100 to 500 mM, and the roughness increases with a further increase in the concentration of AgNO3. The EMI shielding effectiveness (SE) of the film is measured in the frequency range of 0.045 to 1 GHz. As a result of optimizing the electrical conductivity by measuring sheet resistance of the thin silver layer, the film fabricated from 500 mM AgNO3 exhibits the highest EMI SE among all fabricated films. The maximum values of the EMI SE are 60.490 dB at 0.1 GHz and 54.721 dB at 1.0 GHz with minimum sheet resistance of 0.244 Ω/□. Given that the proposed strategy is simple and effective, it is promising for fabricating various low-cost metal films with high EMI SE.

Identification of Unknown Contaminants in Water Samples from ISS Employing Liquid Chromatography/Mass Spectrometry/Mass Spectrometry

NASA Technical Reports Server (NTRS)

Rutz, Jeffrey A.; Schultz, John R.

2008-01-01

Mass Spectrometry/Mass Spectrometry (MS/MS) is a powerful technique for identifying unknown organic compounds. For non-volatile or thermally unstable unknowns dissolved in liquids, liquid chromatography/mass spectrometry/mass spectrometry (LC/MS/MS) is often the variety of MS/MS used for the identification. One type of LC/MS/MS that is rapidly becoming popular is time-of-flight (TOF) mass spectrometry. This technique is now in use at the Johnson Space Center for identification of unknown nonvolatile organics in water samples from the space program. An example of the successful identification of one unknown is reviewed in detail in this paper. The advantages of time-of-flight instrumentation are demonstrated through this example as well as the strategy employed in using time-of-flight data to identify unknowns.

Thin hybrid pixel assembly with backside compensation layer on ROIC

NASA Astrophysics Data System (ADS)

Bates, R.; Buttar, C.; McMullen, T.; Cunningham, L.; Ashby, J.; Doherty, F.; Gray, C.; Pares, G.; Vignoud, L.; Kholti, B.; Vahanen, S.

2017-01-01

The entire ATLAS inner tracking system will be replaced for operation at the HL-LHC . This will include a significantly larger pixel detector of approximately 15 m2. For this project, it is critical to reduce the mass of the hybrid pixel modules and this requires thinning both the sensor and readout chips to about 150 micrometres each. The thinning of the silicon chips leads to low bump yield for SnAg bumps due to bad co-planarity of the two chips at the solder reflow stage creating dead zones within the pixel array. In the case of the ATLAS FEI4 pixel readout chip thinned to 100 micrometres, the chip is concave, with the front side in compression, with a bow of +100 micrometres at room temperature which varies to a bow of -175 micrometres at the SnAg solder reflow temperature, caused by the CTE mismatch between the materials in the CMOS stack and the silicon substrate. A new wafer level process to address the issue of low bump yield be controlling the chip bow has been developed. A back-side dielectric and metal stack of SiN and Al:Si has been deposited on the readout chip wafer to dynamically compensate the stress of the front side stack. In keeping with a 3D process the materials used are compatible with Through Silicon Via (TSV) technology with a TSV last approach which is under development for this chip. It is demonstrated that the amplitude of the correction can be manipulated by the deposition conditions and thickness of the SiN/Al:Si stack. The bow magnitude over the temperature range for the best sample to date is reduced by almost a factor of 4 and the sign of the bow (shape of the die) remains constant. Further development of the backside deposition conditions is on-going with the target of close to zero bow at the solder reflow temperature and a minimal bow magnitude throughout the temperature range. Assemblies produced from FEI4 readout wafers thinned to 100 micrometres with the backside compensation layer have been made for the first time and

Low-Dimensional Nanomaterials as Active Layer Components in Thin-Film Photovoltaics

NASA Astrophysics Data System (ADS)

Shastry, Tejas Attreya

Thin-film photovoltaics offer the promise of cost-effective and scalable solar energy conversion, particularly for applications of semi-transparent solar cells where the poor absorption of commercially-available silicon is inadequate. Applications ranging from roof coatings that capture solar energy to semi-transparent windows that harvest the immense amount of incident sunlight on buildings could be realized with efficient and stable thin-film solar cells. However, the lifetime and efficiency of thin-film solar cells continue to trail their inorganic silicon counterparts. Low-dimensional nanomaterials, such as carbon nanotubes and two-dimensional metal dichalcogenides, have recently been explored as materials in thin-film solar cells due to their exceptional optoelectronic properties, solution-processability, and chemical inertness. Thus far, issues with the processing of these materials has held back their implementation in efficient photovoltaics. This dissertation reports processing advances that enable demonstrations of low-dimensional nanomaterials in thin-film solar cells. These low-dimensional photovoltaics show enhanced photovoltaic efficiency and environmental stability in comparison to previous devices, with a focus on semiconducting single-walled carbon nanotubes as an active layer component. The introduction summarizes recent advances in the processing of carbon nanotubes and their implementation through the thin-film photovoltaic architecture, as well as the use of two-dimensional metal dichalcogenides in photovoltaic applications and potential future directions for all-nanomaterial solar cells. The following chapter reports a study of the interaction between carbon nanotubes and surfactants that enables them to be sorted by electronic type via density gradient ultracentrifugation. These insights are utilized to construct of a broad distribution of carbon nanotubes that absorb throughout the solar spectrum. This polychiral distribution is then shown

Determination of nandrolone metabolites in human urine: comparison between liquid chromatography/tandem mass spectrometry and gas chromatography/mass spectrometry.

PubMed

Buiarelli, Francesca; Giannetti, Luigi; Jasionowska, Renata; Cruciani, Claudia; Neri, Bruno

2010-07-15

Nandrolone (19-nortestosterone) is an androgenic anabolic steroid illegally used as a growth-promoting agent in animal breeding and as a performance enhancer in athletics. Therefore, its use was officially banned in 1974 by the Medical Commission of the International Olympic Committee (IOC). Following nandrolone administration, the main metabolites in humans are 19-norandrosterone, 19-norethiocolanolone and 19-norepiandrosterone, and their presence in urine is the basis of detecting its abuse. The present work was undertaken to determine, in human urine, nandrolone metabolites (phase I and phase II) by developing and comparing multiresidue liquid chromatography/tandem mass spectrometry (LC/MS/MS) and gas chromatography/mass spectrometry (GC/MS) methods. A double extraction by solid-phase extraction (SPE) was necessary for the complete elimination of the interfering compounds. The proposed methods were also tested on a real positive sample, and they allow us to determine the conjugated/free fractions ratio reducing the risk of false positive or misleading results and they should allow laboratories involved in doping control analysis to monitor the illegal use of steroids. The advantages of LC/MS/MS over GC/MS (which is the technique mainly used) include the elimination of the hydrolysis and derivatization steps: it is known that during enzymatic hydrolysis several steroids can be converted into related compounds and deconjugation is not always 100% effective. The validation parameters for the two methods were similar (limit of quantification (LOQ) <1 ng/mL and percentage coefficient of variance (CV%) <16.4), and both were able to confirm unambiguously all the analytes, thus confirming the validity of both techniques. Copyright 2010 John Wiley & Sons, Ltd.

Liquid Chromatography Electrospray Ionization Mass Spectrometric (LC-ESI-MS) and Desorption Electrospray Ionization Mass Spectrometric (DESI-MS) Identification of Chemical Warfare Agents in Consumer Products

DTIC Science & Technology

2007-06-01

T ACanadaY Approved for PublicR Distribution Uln& Liquid Chromatography Electrospray Ionization Mass Spectrometric ( LC -ESI- MS) and Desorption...consumer products with chemical warfare agents or other toxic chemicals. Liquid chromatography electrospray ionization mass spectrometry ( LC -ESI-MS) and...house LC -ESI-MS and LC -ESI-MS/MS methods were evaluated for the determination of chemical warfare agents in spiked bottled water samples. The

Effect of Selectively Etched Ferroelectric Thin-Film Layer on the Performance of a Tunable Bandpass Filter

NASA Technical Reports Server (NTRS)

Subramanyam, Guru; Vignesparamoorthy, Sivaruban; Mueller, Carl; VanKeuls, Fred; Warner, Joseph; Miranda, Felix A.

2001-01-01

The main purpose of this work is to study the effect of a selectively etched ferroelectric thin film layer on the performance of an electrically tunable filter. An X-band tunable filter was designed, fabricated and tested on a selectively etched Barium Strontium Titanate (BSTO) ferroelectric thin film layer. Tunable filters with varying lengths of BSTO thin-film in the input and output coupling gaps were modeled, as well as experimentally tested. Experimental results showed that filters with coupling gaps partially filled with BSTO maintained frequency tunability and improved the insertion loss by approx. 2dB. To the best of our knowledge, these results represent the first experimental demonstration of the advantages of selective etching in the performance of thin film ferroelectric-based tunable microwave components.

Hierarchical CaCO3 chromatography: a stationary phase based on biominerals.

PubMed

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.

Quantitation of acrylamide in food products by liquid chromatography/mass spectrometry.

PubMed

Eberhart, B Loye; Ewald, Deborah K; Sanders, Robert A; Tallmadge, Daniel H; Zyzak, David V; Strothers, Melissa A

2005-01-01

A simple and inexpensive liquid chromatography/mass spectrometry (LC/MS) method was developed for the quantitation of acrylamide in various food products. The method involved spiking the isotope-substituted internal standard (1-C13 acrylamide) onto 6.00 g of the food product, adding 40 mL distilled/deionized water, and heating at 65 degrees C for 30 min. Afterwards, 10 mL ethylene dichloride was added and the mixture was homogenized for 30 s and centrifuged at 2700 x g for 30 min, and then 8 g supernatant was extracted with 10, 5, and 5 mL portions of ethyl acetate. The extracts were combined, dried with sodium sulfate, and concentrated to 100-200 microL. Acrylamide was determined by analysis of the final extract on a single quadrupole, bench-top mass spectrometer with electrospray ionization, using a 2 mm id C18 column and monitoring m/z = 72 (acrylamide) and m/z = 73 (internal standard). For difficult food matrixes, such as coffee and cocoa, a solid-phase extraction cleanup step was incorporated to improve both chromatography and column lifetime. The method had a limit of quantitation of 10 ppb, and coefficients of determination (r2) for calibration curves were typically better than 0.998. Acceptable spike recovery results were achieved in 11 different food matrixes. Precision in potato chip analyses was 5-8% (relative standard deviation). This method provides an LC/MS alternative to the current LC/MS/MS methods and derivatization gas chromatography/mass spectrometry methods, and is applicable to difficult food products such as coffee, cocoa, and high-salt foods.

The properties of plasma-enhanced atomic layer deposition (ALD) ZnO thin films and comparison with thermal ALD

NASA Astrophysics Data System (ADS)

Kim, Doyoung; Kang, Hyemin; Kim, Jae-Min; Kim, Hyungjun

2011-02-01

Zinc oxide (ZnO) thin films were prepared by plasma-enhanced atomic layer deposition (PE-ALD) using oxygen plasma as a reactant and the properties were compared with those of thermal atomic layer deposition (TH-ALD) ZnO thin films. While hexagonal wurzite phase with preferential (0 0 2) orientation was obtained for both cases, significant differences were observed in various aspects of film properties including resistivity values between these two techniques. Photoluminescence (PL) measurements have shown that high resistivity of PE-ALD ZnO thin films is due to the oxygen interstitials at low growth temperature of 200 °C, whose amount decreases with increasing growth temperature. Thin film transistors (TFT) using TH- and PE-ALD ZnO as an active layer were also fabricated and the device properties were evaluated comparatively.

Determination of formetanate hydrochloride in fruit samples using liquid chromatography-mass selective detection or -tandem mass spectrometry.

PubMed

Podhorniak, Lynda V; Kamel, Alaa; Rains, Diane M

2010-05-26

A rapid multiresidue method that captures residues of the insecticide formetanate hydrochloride (FHCl) in selected fruits is described. The method was used to provide residue data for dietary exposure determinations of FHCl. Using an acetonitrile extraction with a dispersive cleanup based on AOAC International method 2007.01, also known as QuEChERS, which was further modified and streamlined, thousands of samples were successfully analyzed for FHCl residues. FHCl levels were determined both by liquid chromatography-single-stage mass spectrometry (LC-MS) and ultraperformance liquid chromatography (UPLC)-tandem mass spectrometry (LC-MS/MS). The target limit of detection (LOD) and the limit of quantitation (LOQ) achieved for FHCl were 3.33 and 10 ng/g, respectively, with LC-MS and 0.1 and 0.3 ng/g, respectively, with LC-MS/MS. Recoveries at these previously unpublished levels ranged from 95 to 109%. A set of 20-40 samples can be prepared in one working day by two chemists.

Comparison of precursor infiltration into polymer thin films via atomic layer deposition and sequential vapor infiltration using in-situ quartz crystal microgravimetry

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

Padbury, Richard P.; Jur, Jesse S., E-mail: jsjur@ncsu.edu

Previous research exploring inorganic materials nucleation behavior on polymers via atomic layer deposition indicates the formation of hybrid organic–inorganic materials that form within the subsurface of the polymer. This has inspired adaptations to the process, such as sequential vapor infiltration, which enhances the diffusion of organometallic precursors into the subsurface of the polymer to promote the formation of a hybrid organic–inorganic coating. This work highlights the fundamental difference in mass uptake behavior between atomic layer deposition and sequential vapor infiltration using in-situ methods. In particular, in-situ quartz crystal microgravimetry is used to compare the mass uptake behavior of trimethyl aluminummore » in poly(butylene terephthalate) and polyamide-6 polymer thin films. The importance of trimethyl aluminum diffusion into the polymer subsurface and the subsequent chemical reactions with polymer functional groups are discussed.« less

Effect of native oxide layers on copper thin-film tensile properties: A reactive molecular dynamics study

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

Skarlinski, Michael D., E-mail: michael.skarlinski@rochester.edu; Quesnel, David J.; Department of Mechanical Engineering, University of Rochester, Rochester, New York 14627

2015-12-21

Metal-oxide layers are likely to be present on metallic nano-structures due to either environmental exposure during use, or high temperature processing techniques such as annealing. It is well known that nano-structured metals have vastly different mechanical properties from bulk metals; however, difficulties in modeling the transition between metallic and ionic bonding have prevented the computational investigation of the effects of oxide surface layers. Newly developed charge-optimized many body [Liang et al., Mater. Sci. Eng., R 74, 255 (2013)] potentials are used to perform fully reactive molecular dynamics simulations which elucidate the effects that metal-oxide layers have on the mechanical propertiesmore » of a copper thin-film. Simulated tensile tests are performed on thin-films while using different strain-rates, temperatures, and oxide thicknesses to evaluate changes in yield stress, modulus, and failure mechanisms. Findings indicate that copper-thin film mechanical properties are strongly affected by native oxide layers. The formed oxide layers have an amorphous structure with lower Cu-O bond-densities than bulk CuO, and a mixture of Cu{sub 2}O and CuO charge character. It is found that oxidation will cause modifications to the strain response of the elastic modulii, producing a stiffened modulii at low temperatures (<75 K) and low strain values (<5%), and a softened modulii at higher temperatures. While under strain, structural reorganization within the oxide layers facilitates brittle yielding through nucleation of defects across the oxide/metal interface. The oxide-free copper thin-film yielding mechanism is found to be a tensile-axis reorientation and grain creation. The oxide layers change the observed yielding mechanism, allowing for the inner copper thin-film to sustain an FCC-to-BCC transition during yielding. The mechanical properties are fit to a thermodynamic model based on classical nucleation theory. The fit implies that the oxidation of

Ultra-high-pressure liquid chromatography-tandem mass spectrometry method for the determination of alkylphenols in soil.

PubMed

Wang, Jing; Pan, Hefang; Liu, Zhengzheng; Ge, Fei

2009-03-20

A novel method has been developed for the determination of alkylphenols in soil by ultra-high-pressure liquid chromatography employing small particle sizes, combined with tandem mass spectrometry. Soil samples were extracted with pressurized liquid extraction (PLE) and then cleaned with solid-phase extraction (SPE). The extracts were separated on C18 column (1.7 microm, 50 mm x 2.1mm) with a gradient elution and a mobile phase consisting of water and acetonitrile, and then detected by an electrospray ionization tandem mass spectrometry in negative ion mode with multiple reaction monitoring (MRM). Compared with traditional liquid chromatography, it took ultra-high-pressure liquid chromatography much less time to analyze alkylphenols. Additionally, the ultra-high-pressure liquid chromatography/tandem mass spectrometry method produces satisfactory reliability, sensitivity, and accuracy. The average recoveries of the three target analytes were 74.0-103.4%, with the RSD<15%. The calibration curves for alkylphenols were linear within the range of 0.01-0.4 microg/ml, with the correlation coefficients greater than 0.99. When 10 g soil sample was used for analysis, the limits of quantification (LOQs) of the three alkylphenols were all 1.0 microg/kg.

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

ERIC Educational Resources Information Center

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…

Polishability of thin electrolytic and electroless NiP layers

NASA Astrophysics Data System (ADS)

Kinast, Jan; Beier, Matthias; Gebhardt, Andreas; Risse, Stefan; Tünnermann, Andreas

2015-10-01

Ultra-precise metal optics are key components of sophisticated scientific instrumentation in astronomy and space applications, covering a wide spectral range. Especially for applications in the visible or ultra-violet spectral ranges, a low roughness of the optics is required. Therefore, a polishable surface is necessary. State of the art is an amorphous nickel-phosphorus (NiP) layer, which enables several polishing techniques achieving a roughness of <1 nm RMS. Typically, these layers are approximately 30 μm to 60 μm thick. Deposited on Al6061, the bimetallic effect leads to a restricted operational temperature, caused by different coefficients of thermal expansion of Al6061 and NiP. Thinner NiP layers reduce the bimetallic effect. Hence, the possible operating temperature range. A deterministic shape correction via Magnetorheological Finishing of the substrate Al6061 leads to low shape deviations prior to the NiP deposition. This allows for depositing thin NiP-layers, which are polishable via a chemical mechanical polishing technique aiming at ultra-precise metal optics. The present article shows deposition processes and polishability of electroless and electrolytic NiP layers with thicknesses between 1 μm and 10 μm.

Thin-Layer Composite Unimorph Ferroelectric Driver Sensor Properties

NASA Technical Reports Server (NTRS)

Mossi, Karla M.; Selby, Gregory V.; Bryant, Robert G.

1998-01-01

Tests were conducted on 13 different configurations of a new class of piezoelectric devices called THUNDER (thin layer composite unimorph ferroelectric driver and sensor). These configurations consisted of a combination of 1, 3, 5, 7, and 9 layers of 25.4 micron thick aluminium as a backing material, with and without a top layer of 25.4 micrometer aluminum. All of these configurations used the same piezoelectric ceramic wafer (PZT-5A) with dimensions of 5.08 x 3.81 x 0.018 cm. The above configurations were tested at two stages of the manufacturing process: before and after repoling. The parameters measured included frequency, driving voltage. displacement, capacitance, and radius of curvature. An optic sensor recorded the displacement at a fixed voltage(100 - 400 V peak to peak) over a predetermined frequency range (1 - 1000 Hz). These displacement measurements were performed using a computer that controlled the process of activating and measuring the displacement of the device. A parameter alpha was defined which can be used to predict the which configuration will produce the most displacement for a free standing device.

Phenolic composition of pomegranate peel extracts using an liquid chromatography-mass spectrometry approach with silica hydride columns.

PubMed

Young, Joshua E; Pan, Zhongli; Teh, Hui Ean; Menon, Veena; Modereger, Brent; Pesek, Joseph J; Matyska, Maria T; Dao, Lan; Takeoka, Gary

2017-04-01

The peels of different pomegranate cultivars (Molla Nepes, Parfianka, Purple Heart, Wonderful and Vkunsyi) were compared in terms of phenolic composition and total phenolics. Analyses were performed on two silica hydride based stationary phases: phenyl and undecanoic acid columns. Quantitation was accomplished by developing a liquid chromatography with mass spectrometry approach for separating different phenolic analytes, initially in the form of reference standards and then with pomegranate extracts. The high-performance liquid chromatography columns used in the separations had the ability to retain a wide polarity range of phenolic analytes, as well as offering beneficial secondary selectivity mechanisms for resolving the isobaric compounds, catechin and epicatechin. The Vkunsyi peel extract had the highest concentration of phenolics (as determined by liquid chromatography with mass spectrometry) and was the only cultivar to contain the important compound punicalagin. The liquid chromatography with mass spectrometry data were compared to the standard total phenolics content as determined by using the Folin-Ciocalteu assay. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.