Extraction and Characterization of Gibberellins from Hordeum vulgare L. Seedlings

1974 ◽  
Vol 1 (2) ◽  
pp. 183 ◽  
Author(s):  
KF Faull ◽  
BG Coombe ◽  
LG Paleg
Keyword(s):  
Mass Spectrometry ◽  
Dry Weight ◽  
Paper Electrophoresis ◽  
The Other ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Fresh Weight ◽  
Hordeum Vulgare L ◽  
Layer Chromatography

Two gibberellins, one GA1-like, the other GA3-like, were identified in the extracts of roots and tops of 8-,11- and 15-day-old barley seedlings by paper chromatography, paper electrophoresis, thin-layer chromatography, gas-liquid chromatography and bioassay procedures, followed by combined gas chromatography-mass spectrometry. The amounts of gibberellins in the seedlings ranged from 7 to 11 ng per plant. The concentrations of gibberellins in the seedlings were 32-320 ng/g dry weight and 5-28 ng/g fresh weight; concentrations in the roots were higher than those in the shoots.

NEUTRAL STEROIDS IN URINE DURING PREGNANCY

1970 ◽  
Vol 65 (1) ◽  
pp. 50-68 ◽  
Author(s):  
O. Jänne ◽  
R. Vihko
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Late Pregnancy ◽  
Paper Electrophoresis ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Pregnant Females ◽  
Urinary Steroids ◽  
Pregnancy Urine ◽  
Layer Chromatography

ABSTRACT A disulphate fraction of the steroids in the urine of pregnant females was separated by chromatography on Sephadex LH-20. The steroids in this fraction showed the mobility of steroid disulphates on thin-layer chromatography, paper chromatography and high-voltage paper electrophoresis. After solvolysis, the free steroids were fractionated on silicic acid and by thin-layer chromatography. Fractions containing dihydroxylated C19 and C21 steroids were obtained. Using gas-liquid chromatography and gas chromatography-mass spectrometry, the following 18 steroids were identified in the disulphate fraction of neutral steroids in late-pregnancy urine: 5α-androstane-3α,17α-diol, androst-5-ene-3β,17α-diol, androst-5-ene-3β,17β-diol, 18-hydroxyandrosterone, 17α-hydroxydehydroepiandrosterone, 16β - hydroxydehydroepiandrosterone, 3β,17β-dihydroxyandrost-5-en-16-one, 5α-pregnane-3α,20α-diol, 5α-pregnane-3β,20α-diol, 5β-pregnane-3α,20α-diol, 5β-pregnane-3β,20α-diol, pregn-5-ene-3β,20α-diol, 3β,16α-dihydroxy-5α-pregnan-20-one, 16α-hydroxypregnenolone, 3α,21-dihydroxy-5α-pregnan-20-one, 3β,21-dihydroxy-5α-pregnan-20-one, 3α,21-dihydroxy-5β-pregnan-20-one and 21-hydroxypregnenolone. 5α-Pregnane-3β,20α-diol was the most abundant steroid in the fraction analysed, and preliminary quantitative data suggest that sulphate-conjugated pregnanediols and 21-hydroxypregnanolones are excreted mainly as disulphates in late pregnancy urine. The origin of these maternal urinary steroids is discussed.

Preparation, isolation, and characterization of permethylated galactosides and fucosides

1999 ◽  
Vol 77 (3) ◽  
pp. 319-325 ◽  
Author(s):  
Daniel D Asres ◽  
Hélène Perreault
Keyword(s):  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Gas Chromatography ◽  
Gas Chromatography Mass Spectrometry ◽  
Characterization Methods ◽  
Isolation And Characterization ◽  
Nmr Data ◽  
Layer Chromatography ◽  
Structural Aspects

Sugar analysis involving permethylation followed by methanolysis can lead to significant results, given that permethylated monosaccharide standards are available for comparison of spectral and chromatographic data. Such standards are not readily commercially available, especially the furanoside forms. This note describes the isolation and characterization of permethylated pyranoside and furanoside species of D(+)-galactose and L(-)-fucose. Separation of the isomers was optimized using a combination of column chromatography and continuous elution thin-layer chromatography (TLC). TLC, gas chromatography - mass spectrometry, and 1H nuclear magnetic resonance (NMR) spectroscopy were used as the characterization methods. The isolation of furanosides is emphasized, since no specific NMR data have been reported on those to date, while several reports have already discussed the structural aspects of pyranosides.Key words: permethylation, monosaccharide, GC-MS, TLC, NMR.

scholarly journals Identification and Characterization of the Genes Involved in Glycosylation Pathways of Mycobacterial Glycopeptidolipid Biosynthesis

2006 ◽  
Vol 188 (1) ◽  
pp. 86-95 ◽  
Author(s):  
Yuji Miyamoto ◽  
Tetsu Mukai ◽  
Noboru Nakata ◽  
Yumi Maeda ◽  
Masanori Kai ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Fatty Acyl ◽  
Gas Chromatography Mass Spectrometry ◽  
Ionization Time ◽  
Flight Mass Spectrometry ◽  
The Common ◽  
Glycosylation Pathway ◽  
Layer Chromatography ◽  
Identification And Characterization

ABSTRACT Glycopeptidolipids (GPLs) are major components present on the outer layers of the cell walls of several nontuberculous mycobacteria. GPLs are antigenic molecules and have variant oligosaccharides in mycobacteria such as Mycobacterium avium. In this study, we identified four genes (gtf1, gtf2, gtf3, and gtf4) in the genome of Mycobacterium smegmatis. These genes were independently inactivated by homologous recombination in M. smegmatis, and the structures of GPLs from each gene disruptant were analyzed. Thin-layer chromatography, gas chromatography-mass spectrometry, and matrix-assisted laser desorption ionization-time-of-flight mass spectrometry analyses revealed that the mutants Δgtf1 and Δgtf2 accumulated the fatty acyl-tetrapeptide core having O-methyl-rhamnose and 6-deoxy-talose as sugar residues, respectively. The mutant Δgtf4 possessed the same GPLs as the wild type, whereas the mutant Δgtf3 lacked two minor GPLs, consisting of 3-O-methyl-rhamnose attached to O-methyl-rhamnose of the fatty acyl-tetrapeptide core. These results indicate that the gtf1 and gtf2 genes are responsible for the early glycosylation steps of GPL biosynthesis and the gtf3 gene is involved in transferring a rhamnose residue not to 6-deoxy-talose but to an O-methyl-rhamnose residue. Moreover, a complementation experiment showed that M. avium gtfA and gtfB, which are deduced glycosyltransferase genes of GPL biosynthesis, restore complete GPL production in the mutants Δgtf1 and Δgtf2, respectively. Our findings propose that both M. smegmatis and M. avium have the common glycosylation pathway in the early steps of GPL biosynthesis but differ at the later stages.

Distribution of sterols in fungi. II. Brassicasterol in Tuber and Terfezia species

1985 ◽  
Vol 31 (12) ◽  
pp. 1127-1130 ◽  
Author(s):  
J. D. Weete ◽  
M. Kulifaj ◽  
C. Montant ◽  
W. R. Nes ◽  
M. Sancholle
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Dry Weight ◽  
The Other ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Fruiting Bodies ◽  
Tuber Species ◽  
Yeastlike Cells ◽  
Nuclear Magnetic

Sterols from ascocarps of Tuber (truffle) and Terfezia species were identified by gas–liquid chromatography, gas chromatography – mass spectrometry, and 1H nuclear magnetic resonance, and the structure of brassicasterol from the yeastlike cells of Taphrina deformans confirmed by 1H nuclear magnetic resonance. Sterols of the fruiting bodies ranged from 1.2 to 2.3 μg/mg dry weight. Ergosterol was the principal sterol of Tuber species which also contained 28–44% brassicasterol depending on the species and source of the sample. Terfezia sp., on the other hand, contained about 98% brassicasterol with only small amounts of ergosterol. Brassicasterol is common to several families of the subdivision Ascomycotina, and to our knowledge has not been reported for a nonascomycetous species.

scholarly journals Massive Occurrence of the Harmful Benthic Dinoflagellate Ostreopsis cf. ovata in the Eastern Adriatic Sea

Toxins ◽  
2019 ◽  
Vol 11 (5) ◽  
pp. 300 ◽  
Author(s):  
Živana Ninčević Gladan ◽  
Jasna Arapov ◽  
Silvia Casabianca ◽  
Antonella Penna ◽  
Giorgio Honsell ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Adriatic Sea ◽  
High Resolution Mass Spectrometry ◽  
Dry Weight ◽  
Elisa Assay ◽  
Fresh Weight ◽  
Taxonomic Methods ◽  
Immunoenzymatic Assay ◽  
Resolution Mass

In September 2015, a massive occurrence of the Ostreopsis species was recorded in central Adriatic Kaštela Bay. In order to taxonomically identify the Ostreopsis species responsible for this event and determine their toxin profile, cells collected in seawater and from benthic macroalgae were analyzed. Conservative taxonomic methods (light microscopy and SEM) and molecular methods (PCR-based assay) allowed the identification of the species Ostreopsis cf. ovata associated with Coolia monotis. The abundance of O. cf. ovata reached 2.9 × 104 cells L−1 in seawater, while on macroalgae, it was estimated to be up to 2.67 × 106 cells g−1 of macroalgae fresh weight and 14.4 × 106 cells g−1 of macroalgae dry weight. An indirect sandwich immunoenzymatic assay (ELISA) and liquid chromatography–high-resolution mass spectrometry (LC-HRMS) were used to determine the toxin profile. The ELISA assay revealed the presence of 5.6 pg palytoxin (PLTX) equivalents per O. cf. ovata cell. LC-HRMS was used for further characterization of the toxin profile, which showed that there were 6.3 pg of the sum of ovatoxins (OVTXs) and isobaric PLTX per O. cf. ovata cell, with a prevalence of OVTXs (6.2 pg cell−1), while the isobaric PLTX concentration was very low (0.1 pg cell−1). Among OVTXs, the highest concentration was recorded for OVTX-a (3.6 pg cell−1), followed by OVTX-b (1.3 pg cell−1), OVTX-d (1.1 pg cell−1), and OVTX-c (0.2 pg cell−1).

Characterization of drug interferences caused by coelution of substances in gas chromatography/mass spectrometry confirmation of targeted drugs in full-scan and selected-ion monitoring modes

1994 ◽  
Vol 40 (2) ◽  
pp. 216-220 ◽  
Author(s):  
A H Wu ◽  
D Ostheimer ◽  
M Cremese ◽  
E Forte ◽  
D Hill
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography Mass Spectrometry ◽  
Spectrometric Analysis ◽  
Targeted Drugs ◽  
Selected Ion Monitoring ◽  
Internal Standards ◽  
Target Drug ◽  
Full Scan ◽  
Chromatographic Mass

Abstract Interference by substances coeluting with targeted drugs is a general problem for gas chromatographic/mass spectrometric analysis of urine. To characterize these interferences, we examined human urine samples containing benzoylecgonine and fluconazole, and other drug combinations including deuterated internal standards that coelute (ISd,c) with target drugs, by selected-ion monitoring (SIM) and full-scan mass spectrometry. We show that, by SIM analysis, detecting the presence of an interferent is dependent on the specific IS used for the assay. When an ISd,c is used, the presence of another coeluting substance (interferent) suggests that the intensity of IS ions is substantially diminished, because the interferent affects both the ISd,c and target drug. When a noncoeluting IS (ISnc) is used, the interferent cannot be discerned unless it coincidently contains one or more of the ions monitored for either the target drug or ISnc. Under full-scan analysis, a coeluting interferent is directly discernable by examining the total ion gas chromatogram.

scholarly journals Identification and Analytical Characterization of a Novel Synthetic Cannabinoid-Type Substance in Herbal Material in Europe

Molecules ◽  
2021 ◽  
Vol 26 (4) ◽  
pp. 793
Author(s):  
Emmanouil D. Tsochatzis ◽  
Joao Alberto Lopes ◽  
Margaret V. Holland ◽  
Fabiano Reniero ◽  
Giovanni Palmieri ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Cannabinoid Receptor ◽  
Analytical Data ◽  
Synthetic Cannabinoids ◽  
Synthetic Cannabinoid ◽  
Gas Chromatography Mass Spectrometry ◽  
New Psychoactive Substances ◽  
Synthetic Cannabinoid Receptor Agonists ◽  
Analytical Laboratories

The rapid diffusion of new psychoactive substances (NPS) presents unprecedented challenges to both customs authorities and analytical laboratories involved in their detection and characterization. In this study an analytical approach to the identification and structural elucidation of a novel synthetic cannabimimetic, quinolin-8-yl-3-[(4,4-difluoropiperidin-1-yl) sulfonyl]-4-methylbenzoate (2F-QMPSB), detected in seized herbal material, is detailed. An acid precursor 4-methyl-3-(4,4-difluoro-1-piperidinylsulfonyl) benzoic acid (2F-MPSBA), has also been identified in the same seized material. After extraction from the herbal material the synthetic cannabimimetic, also referred to as synthetic cannabinoid receptor agonists or “synthetic cannabinoids”, was characterized using gas chromatography-mass spectrometry (GC-MS), 1H, 13C, 19F and 15N nuclear magnetic resonance (NMR) and high-resolution tandem mass spectrometry (HR-MS/MS) combined with chromatographic separation. A cheminformatics platform was used to manage and interpret the analytical data from these techniques.

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