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  • Ionic liquid capillary columns for analysis of multi-component volatiles by gas chromatography-mass spectrometry: performance, selectivity, activity and retention indices.

Ionic liquid capillary columns for analysis of multi-component volatiles by gas chromatography-mass spectrometry: performance, selectivity, activity and retention indices.

Analytical and bioanalytical chemistry (2017-11-12)
Michelle S S Amaral, Philip J Marriott, Humberto R Bizzo, Claudia M Rezende
RESUMEN

This study investigates applications and performance evaluation of SLB-IL60, SLB-IL76 and SLB-IL111 columns, in relation to a DB-Wax column, for the analysis of coffee volatile compounds. Both standards and an authentic coffee sample were analysed, with solid-phase microextraction (SPME) sampling of the latter. A cryofocusing method was applied to improve resolution of the earliest eluting peaks using splitless injection SPME sample analysis. The Grob test was used to verify the inertness and efficiency of the columns, helping to understand the interactions between analytes and stationary phases, particularly toward more polar coffee analytes. A DB-5 column was used only in analysis of n-alkanes and Grob test mixtures as an apolar reference. The evaluated ionic liquid columns showed a moderate acid-base character and low inertness for compounds with hydrogen bond capabilities, especially for the hydroxylated analytes, 2,3-butanediol in the Grob test, and furanones and acids in the coffee standards. The columns exhibiting the best resolution and efficiency were DB-Wax and SLB-IL60, both for samples and standards. Although the DB-Wax column is preferred for analysis of coffee volatiles, due to better inertness, the evaluated ionic liquid columns allowed identification of compounds that were not observed in separations with the Wax-phase column in this work. Among these compounds is 3,4-dimethyl-2,5-furandione, seldom reported in the literature of coffee. Proposed improvement by the manufacturer in the inertness of the columns evaluated in this study may lead to better results; so future versions of IL phases may be better applied in the separation of target analytes, especially those with basic character. Graphical abstract Illustrative representation of the sample (coffee) and the chemical structures of the stationary phases of the ionic liquid capillary columns used as object of study in the present work.

MATERIALES
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, for use with manual holder
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, StableFlex
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 23 ga, StableFlex, for use with autosampler
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, StableFlex, for use with autosampler
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Filtro SPME Polidimetilsiloxano (PDMS), df 100 μm(PDMS, needle size 24 ga, for use with manual holder
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Filtro SPME Polidimetilsiloxano (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 23 ga
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Filtro SPME Polidimetilsiloxano (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 24 ga
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
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SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with autosampler
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
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SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with manual holder
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SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 23 ga
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SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
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SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 24 ga
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SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, StableFlex, for use with manual holder
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Filtro SPME Polidimetilsiloxano (PDMS), df 100 μm(PDMS, for use with manual holder, needle size 23 ga
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
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SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, needle size 24 ga, for use with autosampler
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SPME fiber assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm(PDMS/DVB, for use with autosampler, needle size 23 ga
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Kit de surtido de fibra SPME StableFlex, for use with manual holder
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SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm(PEG, for use with autosampler
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SLB®-IL60 Capillary GC Column, L × I.D. 30 m × 0.25 mm, df 0.20 μm
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SLB®-IL111 Capillary GC Column, L × I.D. 100 m × 0.25 mm, df 0.20 μm
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Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
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Kit de surtido de fibra SPME StableFlex, needle size 23 ga, for use with autosampler
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SPME fiber assortment kit 4, for use with manual holder, size 24 ga