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At least 235 records · Page 13

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NASA NTRS1988

Evidence against the involvement of ionically bound cell wall proteins in pea epicotyl growth

Ionically bound cell wall proteins were extracted from 7 day old etiolated pea (Pisum sativum L. cv Alaska) epicotyls with 3 molar LiCl. Polyclonal antiserum was raised in rabbits against the cell wall proteins. Growth assays showed that treatment of growing region segments (5-7 millimeters) of peas with either dialyzed serum, serum globulin fraction, affinity purified immunoglobulin, or papain-cleaved antibody fragments had no effect on growth. Immunofluorescence microscopy confirmed antibody binding to cell walls and penetration of the antibodies into the tissues. Western blot analysis, immunoassay results, and affinity chromatography utilizing Sepharose-bound antibodies confirmed recognition of the protein preparation by the antibodies. Experiments employing in vitro extension as a screening measure indicated no effect upon extension by antibodies, by 50 millimolar LiCl perfusion of the apoplast or by 3 molar LiCl extraction. Addition of cell wall protein to protease pretreated segments did not restore extension nor did addition of cell wall protein to untreated segments increase extension. It is concluded that, although evidence suggests that protein is responsible for the process of extension, the class(es) of proteins which are extracted from pea cell walls with 3 molar LiCl are probably not involved in this process.

NASA Program Space Biology↗

DOE OSTI2024

PeakQC: A Software Tool for Omics-Agnostic Automated Quality Control of Mass Spectrometry Data

Mass spectrometry is broadly employed to study complex molecular mechanisms in various biological and environmental fields, enabling 'omics' research such as proteomics, metabolomics, and lipidomics. As study cohorts grow larger and more complex with dozens to hundreds of samples, the need for robust quality control (QC) measures through automated software tools becomes paramount to ensure the integrity, high quality, and validity of scientific conclusions from downstream analyses and minimize the waste of resources. Since existing QC tools are mostly dedicated to proteomics, automated solutions supporting metabolomics are needed. To address this need, we developed the software PeakQC, a tool for automated QC of MS data that is independent of omics molecular types (i.e., omics-agnostic). It allows automated extraction and inspection of peak metrics of precursor ions (e.g., errors in mass, retention time, arrival time) and supports various instrumentations and acquisition types, from infusion experiments or using liquid chromatography and/or ion mobility spectrometry front-end separations and with/without fragmentation spectra from data-dependent or independent acquisition analyses. Diagnostic plots for fragmentation spectra are also generated. Here, in this paper, we describe and illustrate PeakQC’s functionalities using different representative data sets, demonstrating its utility as a valuable tool for enhancing the quality and reliability of omics mass spectrometry analyses.

47 OTHER INSTRUMENTATION↗

DOE OSTI2023

Anti-fungal bioactive terpenoids in the bioenergy crop switchgrass (Panicum virgatum) may contribute to ecotype-specific microbiome composition

Abstract Plant derived bioactive small molecules have attracted attention of scientists across fundamental and applied scientific disciplines. We seek to understand the influence of these phytochemicals on rhizosphere and root-associated fungi. We hypothesize that – consistent with accumulating evidence that switchgrass genotype impacts microbiome assembly – differential terpenoid accumulation contributes to switchgrass ecotype-specific microbiome composition. An initial in vitro Petri plate-based disc diffusion screen of 18 switchgrass root derived fungal isolates revealed differential responses to upland- and lowland-isolated metabolites. To identify specific fungal growth-modulating metabolites, we tested fractions from root extracts on three ecologically important fungal isolates – Linnemania elongata, Trichoderma sp. and Fusarium sp. Saponins and diterpenoids were identified as the most prominent antifungal metabolites. Finally, analysis of liquid chromatography-purified terpenoids revealed fungal inhibition structure – activity relationships (SAR). Saponin antifungal activity was primarily determined by the number of sugar moieties – saponins glycosylated at a single core position were inhibitory whereas saponins glycosylated at two core positions were inactive. Saponin core hydroxylation and acetylation were also associated with reduced activity. Diterpenoid activity required the presence of an intact furan ring for strong fungal growth inhibition. These results inform future breeding and biotechnology strategies for crop protection with reduced pesticide application.

09 BIOMASS FUELS↗

NASA NTRS1991

NASA Li/CF(x) cell problem analysis: Anion exchange chromatography analysis

An analysis was made of wiper samples used to wipe down lithium/chlorine fluorine battery components and production equipment. These components and equipment were potentially exposed to thionyl chloride vapors. In the presence of moisture, thionyl chloride decomposes to sulfur dioxide and hydrogen chloride. The wiper samples were analyzed for soluble chlorides and fluorides by anion exchange chromatography. During the examination of the test chromatographs, fluoride contamination was discovered in wiper samples from the test equipment. An analytical method to determine fluoride was developed. The first 3 extracts from the potentially exposed and clean wiper samples were tested, and the total fluoride from both groups determined. A comparison of the results from both groups was made to determine the extent of fluoride contamination.

Bytella, Joseph↗

DOE OSTI2023

Advanced Mineral Separations with Novel Simulated Moving Beds

Lithium is a critical mineral that is widely used in batteries and energy storage applications, making it increasingly important in the next few decades. To meet the growing demand for lithium and secure domestic supply chains, there is a need to exploit unconventional lithium resources. However, utilizing current lithium extraction processes is challenging due to the high salinity in those resources. Thus, it is essential to develop energy-efficient, and less chemical-intensive separation processes that can exploit high-salinity lithium resources. Accordingly, this project aims to design a novel zwitterionic stationary phase and use it to develop a continuous chromatography process to recover LiCl minerals from traditionally unexploited domestic saline resources. The developed zwitterionic stationary phase allows fractionating minerals based on their different sorbent affinities under water elution. A systematically designed continuous process can separate lithium from other minerals, reducing the risk of material fouling and the overall chemical consumption to produce battery-grade lithium. This approach is expected to significantly enhance the efficiency and sustainability of the lithium extraction process while also reducing the environmental impact associated with traditional processes. At the end of the project, the technology will be demonstrated in continuous mode using a simulated moving bed (SMB) to recover >100 g of LiCl from real resource waters. The U.S.-based resources that this project targets for LiCl recovery are formation water, oil-produced water, and geothermal brines, supplied by Standard Lithium Ltd. and Shell Inc, respectively.

critical minerals↗

NASA NTRS1992

Novel long-chain anteiso-alkanes and anteiso-alkanoic acids in Antarctic rocks colonized by living and fossil cryptoendolithic microorganisms

Saponified extracts of rock samples colonized by cryptoendolithic microbial communities from the McMurdo Dry Valleys of Southern Victoria Land, Antarctica, were separated into hydrocarbon and fatty acid fractions by silica gel column chromatography. Hydrocarbons and methyl esters of fatty acids were analyzed by capillary gas chromatography-mass spectrometry. Unusually, a suite of long-chain anteiso-alkanes (a-C20 to a-C30) and anteiso-alkanoic acids (a-C20 to a-C30) were detected in many samples, together with straight-chain, branched and/or cyclic and acyclic isoprenoid compounds. These novel compounds are probably derived from unidentified heterotrophic bacteria or symbiotic processes in a unique microbial community in the Antarctic cold desert and suggest the occurrence of a special biosynthetic pathway. Long-chain anteiso-alkanes are probably formed through microbial decarboxylation of corresponding anteiso-alkanoic acids. They may serve as new biomarkers in environmental and geochemical studies.

NASA Program Exobiology↗

DOE OSTI2021

Liquid Chromatography Coupled to Refractive Index or Mass Spectrometric Detection for Metabolite Profiling in Lysate-based Cell-free Systems

Engineering cellular metabolism for targeted biosynthesis can require extensive design-build-test-learn (DBTL) cycles as the engineer works around the cell's survival requirements. Alternatively, carrying out DBTL cycles in cell-free environments can accelerate this process and alleviate concerns with host compatibility. A promising approach to cell-free metabolic engineering (CFME) leverages metabolically active crude cell extracts as platforms for biomanufacturing and for rapidly discovering and prototyping modified proteins and pathways. Realizing these capabilities and optimizing CFME performance requires methods to characterize the metabolome of lysate-based cell-free platforms. That is, analytical tools are necessary for monitoring improvements in targeted metabolite conversions and in elucidating alterations to metabolite flux when manipulating lysate metabolism. In this work, metabolite analyses using high-performance liquid chromatography (HPLC) coupled with either optical or mass spectrometric detection were applied to characterize metabolite production and flux in E. coli S30 lysates. Specifically, this report describes the preparation of samples from CFME lysates for HPLC analyses using refractive index detection (RID) to quantify the generation of central metabolic intermediates and by-products in the conversion of low-cost substrates (i.e., glucose) to various high-value products. The analysis of metabolite conversion in CFME reactions fed with 13 C-labeled glucose through reversed-phase liquid chromatography coupled to tandem mass spectrometry (MS/MS), a powerful tool for characterizing specific metabolite yields and lysate metabolic flux from starting materials, is also presented. Altogether, applying these analytical methods to CFME lysate metabolism enables the advancement of these systems as alternative platforms for executing faster or novel metabolic engineering tasks.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2005

In situ Analysis of Organic Compounds on Mars using Chemical Derivatization and Gas Chromatography Mass Spectrometry

One of the core science objectives of NASA's 2009 Mars Science Laboratory (MSL) mission is to determine the past or present habitability of Mars. The search for key organic compounds relevant to terrestrial life will be an important part of that assessment. We have developed a protocol for the analysis of amino acids and carboxylic acids in Mars analogue materials using gas chromatography mass spectrometry (GCMS). As shown, a variety of carboxylic acids were readily identified in soil collected from the Atacama Desert in Chile at part-per-billion levels by GCMS after extraction and chemical derivatization using the reagent N,N-tert.-butyl (dimethylsilyl) trifluoroacetamide (MTBSTFA). Several derivatized amino acids including glycine and alanine were also detected by GCMS in the Atacama soil at lower concentrations (chromatogram not shown). Lacking derivatization capability, the Viking pyrolysis GCMS instruments could not have detected amino acids and carboxylic acids, since these non-volatile compounds require chemical transformation into volatile species that are stable in a GC column. We are currently optimizing the chemical extraction and derivatization technique for in situ GCMS analysis on Mars. Laboratory results of analyses of Atacama Desert samples and other Mars analogue materials using this protocol will be presented.

Glavin, D. P.↗

NASA NTRS2009

Extraterrestrial Amino Acids in the Almahata Sitta Meteorite

Amino acid analysis of a meteorite fragment of asteroid 2008 TC(sub 3) called Almahata Sitta was carried out using reverse-phase high-perfo rmance liquid chromatography coupled with UV fluorescence detection a nd time-of-flight mass spectrometry (HPLC-FD/ToF-MS) as part of a sam ple analysis consortium. HPLC analyses of hot-water extracts from the meteorite revealed a complex distribution of two- to six-carbon aliph atic amino acids and one- to three carbon amines with abundances rang ing from 0.5 to 149 parts-per-billion (ppb). The enantiomeric ratios of the amino acids alanine, Beta-amino-n-butyric acid (Beta-ABA), 2-amino-2- methylbutanoic acid (isovaline), and 2-aminopentanoic acid (no rvaline) in the meteorite were racemic (D/L approximately 1), indicat ing that these amino acids are indigenous to the meteorite and not te rrestrial contaminants. Several other non-protein amino acids were also identified in the meteorite above background levels including alpha -aminoisobutyric acid (alpha-AIB), 4-amino-2- methybutanoic acid, 4-a mino-3-methylbutanoic acid, and 3-, 4-, and 5-aminopentanoic acid. Th e total abundances of isovaline and AlB in Almahata Sitta are approximately 1000 times lower than the abundances of these amino acids found in the CM carbonaceous meteorite Murchison. The extremely love abund ances and unusual distribution of five carbon amino acids in Almahata Sitta compared to Cl, CM, and CR carbonaceous meteorites and may be due to extensive thermal alteration of amino acids on the parent aster oid by partial melting during formation or impact shock heating.

Glavin, Daniel P.↗

DOE OSTI2022

Analysis, identification and confirmation of synthetic opioids using chloroformate chemistry: Retrospective detection of fentanyl and acetylfentanyl in urine and plasma samples by EI-GC-MS and HR-LC-MS

Electron Impact Gas Chromatography-Mass Spectrometry (EI-GC-MS) and High Resolution Liquid Chromatography-Mass Spectrometry (HR-LC-MS) have been used in the analysis of products arising from the trichloroethoxycarbonylation of fentanyl and acetylfentanyl in urine and plasma matrices. The method involves the initial extraction of both synthetic opioids separately from the matrices followed by detection of the unique products that arise from their reaction with 2,2,2-trichloroethoxycarbonyl chloride (Troc-Cl), namely Troc-norfentanyl and Troc-noracetylfentanyl. The optimized protocol was successfully evaluated for its efficacy at detecting these species formed from fentanyl and acetylfentanyl when present at low and high levels in urine (fentanyl: 5 and 10 ng/mL and acetylfentanyl: 20 and 100 ng/mL) and plasma (fentanyl: 10 and 20 ng/mL and acetylfentanyl: 50 and 200 ng/mL), values that reflect levels reported in overdose victims. The HR-LC-MS method’s LOQ (limit of quantitation) for the Troc-norfentanyl and Troc-noracetylfentanyl products was determined to be ~10 ng/mL for both species. Even though the superiority in the detection of these species by HR-LC-MS over EI-GC-MS, the latter method proved to be important in the detection of the second product from the reaction, namely 2-phenylethyl chloride that is crucial in the determination of the original opioid. This observation highlights the importance of using complimentary analytical techniques in the analysis of a sample, whether biological or environmental in nature. The method herein serves as a complementary, qualitative confirmation for the presence of a fentanyl in collected urine, plasma and by extension other biological samples amenable to the common extraction procedures described for opioid analysis. More importantly, the method’s main strength comes from its ability to react with unknown fentanyls to yield products that can be not only detected by EI-GC-MS and HR-LC-MS but can then be used to retrospectively identify an unknown fentanyl.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1972

A new approach to the isolation of milligram amounts of significant geochemical compounds.

The modification of an automatic preparative collection system for gas-liquid chromatography is described that is designed to make the system operational for milligram-scale high-efficiency separations of selected components in a geological sample. The sample in question is an organic extract from the Green River Formation Oil Shale, and the compounds selected are the sterane and triterpane hydrocarbons.

Wszolek, P. C.↗

NASA NTRS1987

Supercritical fluid extraction and characterization of lipids from algae Scenedesmus obliquus

Lipids were extracted from a protein concentrate of green algae (Scenedesmus obliquus), using a one-step supercritical carbon dioxide extraction procedure in presence of ethanol as an entrainer, and were characterized. The compositions of neutral lipids, glycolipids, and phospholipids, separated into individual components by column, thin-layer, and gas-liquid chromatography procedures, are presented. Fatty acid composition patterns indicated that the major fatty acids were 16:0, 16:1, 16:2, 16:3, 16:4, 18:1, 18:2, and 18:3. The lipids of S. obliquus were found to contain relatively high concentrations of polyunsaturated fatty acids and essential fatty acids.

Choi, K. J.↗

NASA NTRS1995

Chemical Sensing of Unexploded Ordnance with the Mobile Underwater Survey System (MUDSS)

The ability to sense explosives residues in the marine environment is a critical tool for identification and classification of underwater unexploded ordnance (UXO). Trace explosives signatures of TNT and DNT have been extracted from multiple sediment samples adjacent to unexploded undersea ordnance at Halifax Harbor, Canada. The ordnance was hurled into the harbor during a massive explosion fifty years earlier, in 1945 after World War II had ended. Laboratory sediment extractions were made using the solid-phase microextraction (SPME) method in seawater, and detection using the Reversal Electron Attachment Detection (READ) technique and, in the case of DNT, a commercial gas-chromatography/mass spectrometer (GC/MS). Results show that, after more than 50 years in the environment, ordnance which appeared to be physically intact gave good explosives signatures at the parts-per-billion level, whereas ordnance which had been cracked open during the explosion gave no signatures at the 10 parts-per-trillion sensitivity level. These measurements appear to provide the first reported data of explosives signatures from undersea UXOs.

Darrach, M. R.↗

NASA NTRS1997

Fullerenes, fulleranes and polycyclic aromatic hydrocarbons in the Allende meteorite

In this paper, we confirm our earlier observations of fullerenes (C60 and C70) in the Allende meteorite (Becker et al., 1994a, 1995). Fullerene C60 was also detected in two separate C-rich (approximately 0.5-1.0%) dark inclusions (Heymann et al., 1987) that were hand picked from the Allende sample. The amounts of C60 detected were approximately 5 and approximately 10 ppb, respectively, which is considerably less than what was detected in the Allende 15/21 sample (approximately 100 ppb; Becker et al., 1994a, 1995). This suggests that fullerenes are heterogeneously distributed in the meteorite. In addition, we present evidence for fulleranes, (C60Hx), detected in separate samples by laser desorption (reflectron) time-of-flight (TOF) mass spectrometry (LDMS). The LDMS spectra for the Allende extracts were remarkably similar to the spectra generated for the synthetic fullerane mixtures. Several fullerane products were synthesized using a Rh catalyst (Becker et al., 1993a) and separated using high-performance liquid chromatography (HPLC). Polycyclic aromatic hydrocarbons (PAHs) were also observed ppm levels) that included benzofluoranthene and corannulene, a cup-shaped molecule that has been proposed as a precursor molecule to the formation of fullerenes in the gas phase (Pope et al., 1993).

NASA Center ARC↗

NASA NTRS2010

Extraterrestrial Amino Acids in the Almahata Sitta Meteorite

Amino acid analysis of a meteorite fragment of asteroid 2008 TC3 called Almahata Sitta was carried out using reverse-phase liquid chromatography coupled with UV fluorescence detection and time-of-flight mass spectrometry (LC-FD/ToF-MS) as part of a sample analysis consortium. LC-FD/ToF-MS analyses of hot-water extracts from the meteorite revealed a complex distribution of two- to seven-carbon aliphatic amino acids and one- to three-carbon amines with abundances ranging from 0.5 to 149 parts-per-billion (ppb). The enantiomeric ratios of the amino acids alanine, R-amino-n-butyric acid (beta-ABA), 2-amino-2-methylbutanoic acid (isovaline), and 2-aminopentanoic acid (norvaline) in the meteorite were racemic (D/L approximately 1), indicating that these amino acids are indigenous to the meteorite and not terrestrial contaminants. Several other non-protein amino acids were also identified in the meteorite above background levels including alpha-aminoisobutyric acid (alpha-AIB), 4-amino-2- methylbutanoic acid, 4-amino-3-methylbutanoic acid, and 3-, 4-, and 5-aminopentanoic acid. The total abundances of isovaline and alpha-AIB in Almahata Sitta are 1000 times lower than the abundances of these amino acids found in the CM carbonaceous chondrite Murchison. The extremely low abundances and unusual distribution of five carbon amino acids in Almahata Sitta compared to Cl, CM, and CR carbonaceous chondrites may reflect extensive thermal alteration of amino acids on the parent asteroid by partial melting during formation or subsequent impact shock heating. It is also possible that amino acids were synthesized by catalytic reactions on the parent body after asteroid 2008 TC3 cooled to lower temperatures.

Glavin, Daniel P.↗

NASA NTRS1997

Trace Explosives Signatures from World War II Unexploded Undersea Ordnance

Trace explosives signatures of TNT and DNT have been extracted from multiple sediment samples adjacent to unexploded undersea ordnance at Halifax Harbor, Canada. The ordnance was hurled into the harbor during a massive explosion fifty years earlier, in 1945 after World War II had ended. Laboratory sediment extractions were made using the solid-phase microextraction (SPME) method in seawater, and detection using the Reversal Electron Attachment Detection (READ) technique and, in the case of DNT, a commercial gas-chromatography/mass spectrometer (GC/MS).

unexploded↗

DOE OSTI2023

Ultrahigh performance LC/FT-MS non-targeted screening for biomass burning organic aerosol with MZmine2 and MFAssignR

In recent years, ultrahigh performance liquid chromatography Fourier transform mass spectrometry (LC/FT-MS) based non-targeted screening (NTS) methods have become increasingly popular for comprehensive analysis of complex organic mixtures. However, applying these methods for environmental complex mixture analysis is challenging due to the extreme complexity of natural samples and a lack of standard samples or surrogates for environmental complex mixtures. Furthermore, limited molecular markers in the databases and insufficient data processing software workflows make the application of these methods more challenging for environmental complex mixtures. In this work, we implement a new NTS data processing workflow to process data collected from ultrahigh performance liquid chromatography and Fourier transform Orbitrap Elite Mass Spectrometry (LC/FT-MS) by combining MZmine2 and MFAssignR, two opensource data processing tools and commercial Mesquite liquid smoke as a surrogate for biomass burning organic aerosol. MZmine2.53 data extraction followed MFAssignR molecular formula assignment offered noise free and highly accurate 1733 individual molecular formulas presented in liquid smoke with 4906 molecular species, including isomers. The results of this new approach were consistent with the results of direct infusion FT-MS analysis confirming its reliability. Over 90% of the molecular formulas presented in mesquite liquid smoke were matched with the molecular formulas of ambient biomass burning organic aerosol. This suggests the potential use of commercial liquid smoke as a surrogate for biomass burning organic aerosol research. Furthermore, the presented method significantly improves the identification of the molecular composition of biomass burning organic aerosol by successfully addressing some of the limitations related to the data analysis and giving a semi quantitative insight into the analysis.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2020

Internal Standards for Quantitative Analysis of Chemical Warfare Agents by the GC/MS Method: Nerve Agents

General conditions and requirements for an internal standard useful in the determination of chemical warfare agents (CWAs) by the method of gas chromatography coupled with mass detection (GC/MS) were defined. The determination is based on a GC/MS analysis of a mixture of a CWA with an internal standard, conversion of the TIC chromatogram to a chromatogram extracted at a particular m / z ratio, and calculation of the CWA concentration from the internal standard concentration, response factor, and chromatographic peak areas. Available internal standards were identified, and they were verified for seven organophosphorus nerve-paralysing agents. Corresponding response factors were determined as a ratio of gradients of the linear functions of the peak area and compound concentration. Linearity, repeatability, and accuracy of the measurements were evaluated. The determination can be performed on all GC/MS systems of the Fire Rescue Service of the Czech Republic (FRS), where no CWA standards are available.

Capoun, Tomas↗