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000057080 0247_ $$2DOI$$a10.1016/j.chroma.2007.05.038
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000057080 084__ $$2WoS$$aBiochemical Research Methods
000057080 084__ $$2WoS$$aChemistry, Analytical
000057080 1001_ $$0P:(DE-HGF)0$$aBabay, P. A.$$b0
000057080 245__ $$aColumn temperature as an active variable in the isocratic, normal-phase high-performance liquid chromatography separation of lipophilic metabolites of nonylphenol ethoxylates
000057080 260__ $$aNew York, NY [u.a.]$$bScience Direct$$c2007
000057080 300__ $$a227 - 236
000057080 3367_ $$0PUB:(DE-HGF)16$$2PUB:(DE-HGF)$$aJournal Article
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000057080 440_0 $$03154$$aJournal of Chromatography A$$v1157$$x0021-9673
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000057080 520__ $$aNormal-phase separation of technical grade nonylphenol (t-NP, about 90% 4-nonylphenol), 4-nonylphenol mono-ethoxylate (4-NP1EO) and 4-nonylphenol di-ethoxylate (4-NP2EO) was assessed, with the inclusion of column temperature as an active variable. The compound 2,4,6-trimethylphenol was evaluated for use as internal standard. Isocratic elution with 2-propanol/hexanes mixtures from an amino-silica column and spectrometric UV detection at 277 nm were employed. Technical nonylphenol presented a significant contribution from unknown substances that eluted with retention times similar to that of 4-NP1EO. GC-MS analysis of the unknowns allowed to identify them as isomers of 2-NP. The response of the system to joint variations in flow rate, eluent composition and column temperature was investigated by means of Doehlert statistical experimental design. A model for retention of the analytes as a function of the experimental variables was proposed, and separation selectivity was studied. Selection of the optimal working zone was made through desirability function (D) calculations. Potential co-elution of 2-NP isomers with 4-NP1EO was considered when optimizing the separation. The occurrence of a restricted region of the experimental space where baseline resolution of analytes, associated impurities and internal standard results feasible (D not equal to 0) is apparent.
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000057080 650_2 $$2MeSH$$aChromatography, High Pressure Liquid: instrumentation
000057080 650_2 $$2MeSH$$aEthylene Glycols: isolation & purification
000057080 650_2 $$2MeSH$$aEthylene Glycols: metabolism
000057080 650_2 $$2MeSH$$aSensitivity and Specificity
000057080 650_2 $$2MeSH$$aSpectrophotometry, Ultraviolet
000057080 650_2 $$2MeSH$$aTemperature
000057080 650_7 $$00$$2NLM Chemicals$$aEthylene Glycols
000057080 650_7 $$027986-36-3$$2NLM Chemicals$$aterics
000057080 650_7 $$2WoSType$$aJ
000057080 65320 $$2Author$$anonylphenol ethoxylates
000057080 65320 $$2Author$$alipophilic metabolites
000057080 65320 $$2Author$$anormal-phase HPLC
000057080 65320 $$2Author$$acolumn temperature
000057080 65320 $$2Author$$aseparation selectivity
000057080 7001_ $$0P:(DE-HGF)0$$aGettar, R. T.$$b1
000057080 7001_ $$0P:(DE-HGF)0$$aMagallanes, J.F.$$b2
000057080 7001_ $$0P:(DE-HGF)0$$aBecquart, E.T.$$b3
000057080 7001_ $$0P:(DE-Juel1)129410$$aThiele, B.$$b4$$uFZJ
000057080 7001_ $$0P:(DE-HGF)0$$aBatistoni, D. A.$$b5
000057080 773__ $$0PERI:(DE-600)1491247-8$$a10.1016/j.chroma.2007.05.038$$gVol. 1157, p. 227 - 236$$p227 - 236$$q1157<227 - 236$$tJournal of chromatography / A$$v1157$$x0021-9673$$y2007
000057080 8567_ $$uhttp://dx.doi.org/10.1016/j.chroma.2007.05.038
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000057080 9141_ $$y2007
000057080 915__ $$0StatID:(DE-HGF)0010$$aJCR/ISI refereed
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