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Predicate | Object |
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rdf:type | |
lifeskim:mentions | |
pubmed:issue |
2
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pubmed:dateCreated |
1996-7-30
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pubmed:abstractText |
A synthetic mixture containing mainly 4'-bromo-4,5,6,7-tetrachlorofluorescein (4'BrTCF, ca. 25% by high-performance liquid chromatography) was prepared by direct bromination of tetrachlorofluorescein in ethanol. The 4'BrTCF was isolated and purified by pH-zone-refining counter-current chromatography (CCC), using two different two-phase solvent systems: diethyl ether-acetonitrile-water (4:1:5,v/v) and ter.-butyl methyl ether-water (1:1,v/v). For each system, the upper organic phase was acidified and used as the stationary phase and the lower aqueous phase was made basic and used as the mobile phase. pH-Zone-refining CCC of two 5-g batches of the crude mixture yielded 1.65 g of 4'BrTCF that was ca. 95% pure by HPLC. For these separations, a commercial counter-current chromatograph was fitted with a pH electrode in a flow cell to record the pH of the effluent "on line,' thereby replacing the tedious and time-consuming manual measurement of the pH of each fraction. Additionally, UV spectra of the effluent were continuously monitored and stored by using a computerized scanning UV-Vis detector equipped with an adjustable short-pathlength flow cell.
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pubmed:language |
eng
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pubmed:journal | |
pubmed:citationSubset |
IM
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pubmed:chemical | |
pubmed:status |
MEDLINE
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pubmed:month |
May
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pubmed:issn |
0021-9673
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pubmed:author | |
pubmed:issnType |
Print
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pubmed:day |
3
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pubmed:volume |
732
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pubmed:owner |
NLM
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pubmed:authorsComplete |
Y
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pubmed:pagination |
283-90
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pubmed:dateRevised |
2009-1-15
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pubmed:meshHeading |
pubmed-meshheading:8653202-Chromatography, High Pressure Liquid,
pubmed-meshheading:8653202-Coloring Agents,
pubmed-meshheading:8653202-Fluoresceins,
pubmed-meshheading:8653202-Food Additives,
pubmed-meshheading:8653202-Hydrogen-Ion Concentration,
pubmed-meshheading:8653202-Magnetic Resonance Spectroscopy,
pubmed-meshheading:8653202-Mass Spectrometry,
pubmed-meshheading:8653202-Spectrophotometry, Ultraviolet
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pubmed:year |
1996
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pubmed:articleTitle |
Isolation of 4'-bromo-4,5,6,7-tetrachlorofluorescein from a synthetic mixture by pH-zone-refining counter-current chromatography with continuous pH monitoring.
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pubmed:affiliation |
Office of Cosmetics and Colors, US Food and Drug Administration, Washington, DC 20204, USA.
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pubmed:publicationType |
Journal Article
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