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Das, P.P.; Guzzinati, G.; Coll, C.; Gomez Perez, A.; Nicolopoulos, S.; Estrade, S.; Peiro, F.; Verbeeck, J.; Zompra, A.A.; Galanis, A.S. |
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Title |
Reliable Characterization of Organic & Pharmaceutical Compounds with High Resolution Monochromated EEL Spectroscopy |
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A1 Journal article |
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Year  |
2020 |
Publication |
Polymers |
Abbreviated Journal |
Polymers-Basel |
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Volume |
12 |
Issue |
7 |
Pages |
1434 |
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Keywords |
A1 Journal article; Electron microscopy for materials research (EMAT) |
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Abstract |
Organic and biological compounds (especially those related to the pharmaceutical industry) have always been of great interest for researchers due to their importance for the development of new drugs to diagnose, cure, treat or prevent disease. As many new API (active pharmaceutical ingredients) and their polymorphs are in nanocrystalline or in amorphous form blended with amorphous polymeric matrix (known as amorphous solid dispersion—ASD), their structural identification and characterization at nm scale with conventional X-Ray/Raman/IR techniques becomes difficult. During any API synthesis/production or in the formulated drug product, impurities must be identified and characterized. Electron energy loss spectroscopy (EELS) at high energy resolution by transmission electron microscope (TEM) is expected to be a promising technique to screen and identify the different (organic) compounds used in a typical pharmaceutical or biological system and to detect any impurities present, if any, during the synthesis or formulation process. In this work, we propose the use of monochromated TEM-EELS, to analyze selected peptides and organic compounds and their polymorphs. In order to validate EELS for fingerprinting (in low loss/optical region) and by further correlation with advanced DFT, simulations were utilized. |
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000556786700001 |
Publication Date |
2020-06-27 |
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ISSN |
2073-4360 |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
3.364 |
Times cited |
6 |
Open Access |
OpenAccess |
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Notes |
C.C., F.P., S.E. acknowledges the Spanish government for projects MAT2016-79455-P, Research Network RED2018-102609-T and the FPI (BES-2017-080045) grant of Ministerio de Ciència, Innovación y Universidades. G.G. acknowledges support from a postdoctoral fellowship grant from the Fonds Wetenschappelijk Onderzoek—Vlaanderen (FWO). P.P.D., A.G.P., S.N. gratefully acknowledge much helpful discussion on EELS study for organic compounds with Dr. Andrey Chuvilin (CIC NANOGUNE, Donostia—San Sebastian, Spain). The authors also acknowledge Raúl Arenal (University de Zaragoza, Spain) for useful discussion on EELS. The authors acknowledge also Ulises Julio Amador Elizondo (Universidad CEU San Pablo, Spain) for kindly provide the aripiprazole and piroxicam samples for EELS study.; EUSMI_TA; |
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Most recent IF: NA |
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Call Number |
EMAT @ emat @c:irua:170603 |
Serial |
6400 |
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Guzzinati, G.; Das, P.P.; Zompra, A., A.; Nicopoulos, S.; Verbeeck, J. |
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Title |
Electron energy loss spectra of several organic compounds |
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Dataset |
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Year |
2020 |
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Dataset; Electron microscopy for materials research (EMAT) |
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We placed crystals of different compounds to explore the possibility of fingerprinting them through EELS. Here are representative datasets of 7 different compounds: b-cyclodextrin hexacarboxy cyclohexane tannin TH-15 peptide TH-27 peptide two different forms of piroxicam The datasets were collected at EMAT, using a monochromated FEI Titan3 TEM, within the scope of an EUSMI request. More information as well as analysis methodologies adopted for the data are detailed in the paper: Das et al. “Reliable Characterization of Organic & Pharmaceutical Compounds with High Resolution Monochromated EEL Spectroscopy”, Polymers 2020, 12(7), 1434. |
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Most recent IF: NA |
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Call Number |
UA @ admin @ c:irua:180654 |
Serial |
6866 |
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Koblischka, M.R.; Winter, M.; Das, P.; Koblischka-Veneva, A.; Muralidhar, M.; Wolf, T.; Babu, N.H.; Turner, S.; Van Tendeloo, G.; Hartmann, U. |
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Title |
Observation of nanostripes and -clusters in (Nd, EuGd)Ba2Cu3Ox superconductors |
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A1 Journal article |
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Year |
2009 |
Publication |
Physica: C : superconductivity |
Abbreviated Journal |
Physica C |
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469 |
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4 |
Pages |
168-176 |
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Keywords |
A1 Journal article; Electron microscopy for materials research (EMAT) |
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Nanostripes are observed in melt-textured and single-crystalline samples of the ternary light rare earth (LRE)-compound (Nd0.33Eu0.33Gd0.33)Ba2Cu3Ox (NEG) by means of atomic force microscopy, scanning tunnelling microscopy at ambient conditions, combined with transmission electron microscopy and electron backscatter diffraction. This enables the observation of several important features: The nanostripes are formed by chains of nanoclusters, representing the LRE/Ba substitution. The dimensions of the nanostripes are similar for both types of NEG samples. The periodicity of the nanostripes is found to range between 40 and 60 nm; the shape of the nanoclusters is elliptic with a major axis length between 300 and 500 nm and a minor axis length of about 30150 nm. The stripes are filling effectively the space in between the twin boundaries. Concerning the flux pinning, the nanoclusters are the important pinning sites, not the nanostripes themselves. |
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Amsterdam |
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000264657100008 |
Publication Date |
2009-01-23 |
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0921-4534; |
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UA library record; WoS full record; WoS citing articles |
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Impact Factor |
1.404 |
Times cited |
6 |
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Most recent IF: 1.404; 2009 IF: 0.723 |
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Call Number |
UA @ lucian @ c:irua:76403 |
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2418 |
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Das, P.; Koblischka, M.R.; Turner, S.; Van Tendeloo, G.; Wolf, T.; Jirsa, M.; Hartmann, U. |
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Title |
Direct observation of nanometer-scale pinning sites in (Nd0.33Eu0.20Gd0.47)Ba2Cu3O7-\delta single crystals |
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A1 Journal article |
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2008 |
Publication |
Europhysics letters |
Abbreviated Journal |
Epl-Europhys Lett |
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83 |
Issue |
3 |
Pages |
37005,1-37005,4 |
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Keywords |
A1 Journal article; Electron microscopy for materials research (EMAT) |
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We report on the observation of self-organized stripe-like structures on the as-grown surface and in the bulk of (Nd,Eu,Gd)Ba2Cu3Oy single crystals. The periodicity of the stripes on the surface lies between 500800 nm. These are possibly the growth steps of the crystal. Transmission electron microscopy investigations revealed stripes of periodicity in the range of 2040 nm in the bulk. From electron back scattered diffraction investigations, no crystallographic misorientation due to the nanostripes has been found. Scanning tunneling spectroscopic experiments revealed nonsuperconducting regions, running along twin directions, which presumably constitute strong pinning sites. |
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Paris |
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000259022600032 |
Publication Date |
2008-07-18 |
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0295-5075;1286-4854; |
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Additional Links |
UA library record; WoS full record; WoS citing articles |
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Impact Factor |
1.957 |
Times cited |
5 |
Open Access |
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Notes |
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Most recent IF: 1.957; 2008 IF: 2.203 |
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Call Number |
UA @ lucian @ c:irua:76496 |
Serial |
719 |
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