scholarly journals Microextraction of Reseda luteola-Dyed Wool and Qualitative Analysis of Its Flavones by UHPLC-UV, NMR and MS

Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3787
Author(s):  
Elbert van der Klift ◽  
Alexandre Villela ◽  
Goverdina C. H. Derksen ◽  
Peter P. Lankhorst ◽  
Teris A. van Beek
Keyword(s):  
Quality Control ◽  
High Resolution ◽  
Chromatographic Analysis ◽  
2D Nmr ◽  
Reversed Phase ◽  
Detailed Knowledge ◽  
Signal To Noise ◽  
Chromatographic Fingerprints ◽  
Good Signal ◽  
First Time

Detailed knowledge on natural dyes is important for agronomy and quality control as well as the fastness, stability, and analysis of dyed textiles. Weld (Reseda luteola L.), which is a source of flavone-based yellow dye, is the focus of this study. One aim was to reduce the required amount of dyed textile to ≤50 μg for a successful chromatographic analysis. The second aim was to unambiguously confirm the identity of all weld flavones. By carrying out the extraction of 50 μg dyed wool with 25 μL of solvent and analysis by reversed-phase UHPLC at 345 nm, reproducible chromatographic fingerprints could be obtained with good signal to noise ratios. Ten baseline separated peaks with relative areas ≥1% were separated in 6 min. Through repeated polyamide column chromatography and prepHPLC, the compounds corresponding with the fingerprint peaks were purified from dried weld. Each was unequivocally identified, including the position and configuration of attached sugars, by means of 1D and 2D NMR and high-resolution MS. Apigenin-4′-O-glucoside and luteolin-4′-O-glucoside were additionally identified as two trace flavones co-eluting with other flavone glucosides, the former for the first time in weld. The microextraction might be extended to other used dye plants, thus reducing the required amount of precious historical textiles.

Fully-Automated Synthesis of 177Lu Labelled FAPI Derivatives On The Module Modular Lab-Eazy

2021 ◽  
Author(s):  
Kurtulus Eryilmaz ◽  
Benan KILBAS
Keyword(s):  
Quality Control ◽  
Chromatographic Analysis ◽  
Radiochemical Purity ◽  
Radiochemical Yield ◽  
Automated System ◽  
Automated Synthesis ◽  
Modular Approach ◽  
Stability Studies ◽  
European Pharmacopoeia ◽  
First Time

Abstract Backround: To the best of our knowledge, manually production of [177Lu]Lu-FAPI radiopharmaceutical derivatives has been only described in literature. In this work, a fully-automated [177Lu]Lu-FAPI synthesis has been well designed for the first time using commercially available synthesis module. In addition to the development of an automated system with disposable cassette, quality control (QC) and stability studies were comprehensively employed. Results A fully automated synthesis of [177Lu]Lu-FAPI derivatives was achieved on the Modular Lab Eazy (ML Eazy) with high radiochemical yield (85–90%). Chromatographic analysis indicated the formation of radiosynthesis with an absolute radiochemical purity (99%). Stability experiments clarified the durability of the products within 4 days. All obtained specifications are consistent to European Pharmacopoeia. Conclusion A fully automated synthesis of [177Lu]Lu-FAPI radiopharmaceuticals were accomplished regarding quality control standards and quality assurance by using commercially available a modular approach namely ML Eazy with disposable customized cassette and template.

A Study of the Orbital and Intrinsic Variability of the Double-Lined Spectroscopic Binary β Centauri

2002 ◽  
Vol 185 ◽  
pp. 86-87
Author(s):  
M. Ausseloos ◽  
C. Aerts ◽  
K. Uytterhoeven
Keyword(s):  
High Resolution ◽  
Orbital Motion ◽  
High Signal ◽  
Mass Ratio ◽  
Eccentric Orbit ◽  
Intrinsic Variability ◽  
Signal To Noise ◽  
Orbital Parameters ◽  
Spectroscopic Binary ◽  
First Time

AbstractWe introduce our observational study of the orbital motion of β Cen. Using 463 high signal-to-noise, high-resolution spectra obtained over a timespan of 12 years it is shown that the radial velocity of β Cen varies with an orbital period of 357.0 days. We derive for the first time the orbital parameters of β Cen and find a very eccentric orbit (e = 0.81) and similar component masses with a mass ratio M1/M2 = 1.02. Both the primary and the secondary exhibit periodic line-profile variations.

scholarly journals The well correlated diffuse interstellar bands at λλ 6196, 6614 Å and their possible companions

2020 ◽  
Vol 496 (2) ◽  
pp. 2231-2240
Author(s):  
A Bondar
Keyword(s):  
Polycyclic Aromatic Hydrocarbons ◽  
High Resolution ◽  
Aromatic Hydrocarbons ◽  
Correlation Coefficients ◽  
High Signal ◽  
Signal To Noise ◽  
B Stars ◽  
Diffuse Interstellar Bands ◽  
Polycyclic Aromatic ◽  
First Time

ABSTRACT Considered here is the interrelation between five diffuse interstellar bands (DIBs), λλ 5545, 6113, 6196, 6445 and 6614 Å. Two DIBs (λλ 6196 and 6614 Å) are already known as being well correlated with each other; their relation with three other weaker bands is investigated for the first time. To accomplish this task, high-resolution spectra (λ/δλ ≈100 000) with high signal-to-noise ratios (S/N) of 54 hot O–B stars with reddening 0.12–1.45 mag were used. Analysis of measured equivalent widths has allowed us to establish linear dependences and evaluate linear correlation coefficients as high as 0.968–0.988 between the intensities of these five DIBs. Such a degree of correlation may indicate their common origin. Several spacings in wavenumbers found between these DIBs correspond to the energies of vibrational transitions in some polycyclic aromatic hydrocarbons resulting in IR emissions at λλ 16.4, 11.3, 7.7, 6.2 and 3.3 μm.

scholarly journals Chasing the Major Sphingolipids on Earth: Automated Annotation of Plant Glycosyl Inositol Phospho Ceramides by Glycolipidomics

Metabolites ◽  
2020 ◽  
Vol 10 (9) ◽  
pp. 375 ◽  
Author(s):  
Lisa Panzenboeck ◽  
Nina Troppmair ◽  
Sara Schlachter ◽  
Gunda Koellensperger ◽  
Jürgen Hartler ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
High Resolution ◽  
High Resolution Mass Spectrometry ◽  
Decision Rules ◽  
Reversed Phase ◽  
Plant Sample ◽  
Automated Annotation ◽  
Plant Samples ◽  
First Time

Glycosyl inositol phospho ceramides (GIPCs) are the major sphingolipids on earth, as they account for a considerable fraction of the total lipids in plants and fungi, which in turn represent a large portion of the biomass on earth. Despite their obvious importance, GIPC analysis remains challenging due to the lack of commercial standards and automated annotation software. In this work, we introduce a novel GIPC glycolipidomics workflow based on reversed-phase ultra-high pressure liquid chromatography coupled to high-resolution mass spectrometry. For the first time, automated GIPC assignment was performed using the open-source software Lipid Data Analyzer (LDA), based on platform-independent decision rules. Four different plant samples (salad, spinach, raspberry, and strawberry) were analyzed and the results revealed 64 GIPCs based on accurate mass, characteristic MS2 fragments and matching retention times. Relative quantification using lactosyl ceramide for internal standardization revealed GIPC t18:1/h24:0 as the most abundant species in all plants. Depending on the plant sample, GIPCs contained mainly amine, N-acetylamine or hydroxyl residues. Most GIPCs revealed a Hex-HexA-IPC core and contained a ceramide part with a trihydroxylated t18:0 or a t18:1 long chain base and hydroxylated fatty acid chains ranging from 16 to 26 carbon atoms in length (h16:0–h26:0). Interestingly, four GIPCs containing t18:2 were observed in the raspberry sample, which was not reported so far. The presented workflow supports the characterization of different plant samples by automatic GIPC assignment, potentially leading to the identification of new GIPCs. For the first time, automated high-throughput profiling of these complex glycolipids is possible by liquid chromatography-high-resolution tandem mass spectrometry and subsequent automated glycolipid annotation based on decision rules.

scholarly journals Flavonoids from Lonchocarpus muehlbergianus

2004 ◽  
Vol 76 (4) ◽  
pp. 651-661 ◽  
Author(s):  
Aderbal F. Magalhães ◽  
Ana M.G.A. Tozzi ◽  
Eva G. Magalhães ◽  
Ivani S. Blanco ◽  
Maria-Del-Pilar C. Soriano
Keyword(s):  
Quantitative Analysis ◽  
Spectral Data ◽  
13C Nmr ◽  
2D Nmr ◽  
Reversed Phase ◽  
Light Petroleum ◽  
Natural Occurrence ◽  
Reversed Phase Hplc ◽  
First Time

The light petroleum extract from the roots of Lonchocarpus muehlbergianus Hassl contained nine flavonoids, including six new ones. These are 2,4-cis-2,4,5,8-tetramethoxy-(2´´,3´´:6,7)-furanoflavan; 2,4-cis-4-hydroxy-2,5,8-trimethoxy-(2´´,3´´:6,7)-furanoflavan; 2,4-cis-2-prenyloxy-4,5,8-trimethoxy-(2´´,3´´:6,7)-fu-ranoflavan; 2,4-cis-2-prenyloxy-4-hydroxy-5,8-dimethoxy-(2´´,3´´:6,7)-furanoflavan; 2',5',6'-trimethoxy-9-(1,1-dimethylallyoxy)-[2´´,3´´:3´,4´]-furanochalcone; 5,6-dimethoxy-(2´´,3´´:7,8)-furanoflavone, identi-fied by analysis of their spectral data (UV, IR, ¹H and 13C NMR, 2D-NMR, NOE and MS). The natural occurrence of 2,4-dioxygenated flavan derivatives is being reported for the first time. Quantitative analysis of the petrol extract, by using reversed-phase HPLC, showed that the most abundant flavonoid in the extract is 2,4-cis-2,4,5,8- tetramethoxy-(2´´,3´´:6,7)-furanoflavan.

Spiral CT of the pancreas

1998 ◽  
Vol 39 (1) ◽  
pp. 60-63 ◽  
Author(s):  
T. Nishiharu ◽  
Y. Yamashita ◽  
I. Ogata ◽  
S. Sumi ◽  
K. Mitsuzaki ◽  
...  
Keyword(s):  
High Resolution ◽  
Spatial Resolution ◽  
High Spatial Resolution ◽  
Signal To Noise Ratio ◽  
Spiral Ct ◽  
Reconstruction Technique ◽  
Signal To Noise ◽  
Standard Size ◽  
Noise Ratio ◽  
Good Signal

Purpose: to compare the value of a retrospective targeted high-resolution spiral CT to the standard reconstruction technique in the assessment of pancreatic diseases Material and Methods: Spiral CT pancreatic images of a standard-size reconstruction protocol were compared prospectively with those of a retrospective targeted high-spatial-resolution reconstruction protocol in 30 patients. Prior to clinical evaluation, a phantom study was performed to evaluate the spatial resolution and signal-to-noise ratio of both protocols Results: the high-resolution protocol achieved a good signal-to-noise ratio with acceptable spatial resolution. Phantom studies revealed increased image noise (+17%) with an increase in spatial resolution (+100%). in patients studied with the high-resolution protocol, the increase in noise was not significant but there was a marked improvement in the definition of small details Conclusion: Images obtained with a targeted high-spatial-resolution reconstruction protocol showed superior lesion definition and vascular opacification compared with those obtained with a standard-size reconstruction protocol. This technique may have potential in the evaluation of small pancreatic abnormalities

scholarly journals Fully-automated synthesis of 177Lu labelled FAPI derivatives on the module modular lab-Eazy

2021 ◽  
Vol 6 (1) ◽  
Author(s):  
Kurtulus Eryilmaz ◽  
Benan Kilbas
Keyword(s):  
Quality Control ◽  
Chromatographic Analysis ◽  
Radiochemical Purity ◽  
Radiochemical Yield ◽  
Automated System ◽  
Automated Synthesis ◽  
Modular Approach ◽  
Stability Studies ◽  
European Pharmacopoeia ◽  
First Time

Abstract Background To the best of our knowledge, manually production of [177Lu]Lu-FAPI radiopharmaceutical derivatives has been only described in literature. In this work, a fully-automated [177Lu]Lu-FAPI synthesis has been well designed for the first time using commercially available synthesis module. In addition to the development of an automated system with disposable cassette, quality control (QC) and stability studies were comprehensively presented. Results A fully automated synthesis of [177Lu]Lu-FAPI derivatives was achieved on the Modular Lab Eazy (ML Eazy) with high radiochemical yield ([177Lu]Lu-FAPI-04; 88% ± 3, [177Lu]Lu-FAPI-46; 86% ± 3). Chromatographic analysis indicated the formation of radiosynthesis with an absolute radiochemical purity (99%). Stability experiments clarified the durability of the products within 4 days. All obtained specifications are consistent to European Pharmacopoeia. Conclusion A fully automated synthesis of [177Lu]Lu-FAPI radiopharmaceuticals was accomplished regarding quality control standards and quality assurance by using commercially available a modular approach namely ML Eazy with disposable customized cassette and template. Graphical abstract

Two new taxane-glycosides from the needles of Taxus canadensis

2015 ◽  
Vol 70 (11) ◽  
pp. 829-835 ◽  
Author(s):  
Nan Li ◽  
Jin Wang ◽  
Hui-Min Yan ◽  
Man-li Zhang ◽  
Qing-Wen Shi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Data Analysis ◽  
High Resolution ◽  
Fast Atom Bombardment ◽  
2D Nmr ◽  
Taxus Canadensis ◽  
Nmr Data ◽  
First Time

AbstractTwo minor taxane glycosides were isolated for the first time from the needles of Taxus canadensis. Their structures were characterized as 2α,5α-diacetoxy-10β-(6′-O-acetyl-β-d-glucopyranosyl)oxy-14β-[(2′R,3′S)-3′-hydroxy-2′-methylbutanoyl]oxytaxa-4(20),11-diene (1) and 2α,14β-diacetoxy-10β-(β-d-glucopyranosyl)oxytaxa-4(20),11-dien-5β-ol (2) on the basis of 1D and 2D NMR data analysis and confirmed by high-resolution fast atom bombardment mass spectrometry.

scholarly journals Two New 11(15→1)Abeotaxanes with a 2,20-Epoxy Ring from the Needles of Taxus canadensis

2009 ◽  
Vol 64 (1-2) ◽  
pp. 43-48 ◽  
Author(s):  
Man-Li Zhang ◽  
Jing Zhang ◽  
Mei Dong ◽  
Shu-Hua Feng ◽  
Chang-Hong Huo ◽  
...  
Keyword(s):  
High Resolution ◽  
2D Nmr ◽  
Epoxy Ring ◽  
Taxus Canadensis ◽  
Growth Inhibitory ◽  
Weak Growth ◽  
Inhibitory Activities ◽  
First Time

1Two 11(15→1)abeotaxanes having a tetrahydrofuran ring along the carbon atoms C-2, C-3, C-4, C-20 were identified for the first time from the needles of the Canadian yew, Taxus canadensis. The compounds could be identified as 4α,10β,13α-triacetoxy-15-benzoyloxy-2α,20β- epoxy-11(15→1)abeotax-11-ene-5α,7β,9α-triol () and 4α,7β,9α,10β,15-pentaacetoxy-2α,20β- epoxy-11(15→1)abeotax-11-ene-5α,13α-diol (2) on the basis of 1D-, 2D-NMR evidence and high-resolution FABMS analysis. Compound 1 showed weak growth inhibitory activities against T-98 and MM1-CB cells in vitro.

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