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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
ABSTRACT

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.

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Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
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Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray hub
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Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub
Supelco
Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub
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Unità fibra SPME polidimetilsilossano (PDMS), 100 μm PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, red hub
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Gruppo in fibra SPME divinilbenzene/carbossene/polidimetilsilossano (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub
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Unità fibra SPME polidimetilsilossano (PDMS), 100 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, red hub
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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub
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Unità fibra SPME polidimetilsilossano (PDMS), 100 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, red hub
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Gruppo fibre SPME polidimetilsilossano/divinilbenzene (PDMS/DVB), 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, blue hub
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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, light blue hub
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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, black hub
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Gruppo fibre SPME polidimetilsilossano/divinilbenzene (PDMS/DVB), 65 μm PDMS/DVB, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, pink hub
Supelco
Gruppo fibre SPME polidimetilsilossano/divinilbenzene (PDMS/DVB), 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, blue hub
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Gruppo fibre SPME polidimetilsilossano/divinilbenzene (PDMS/DVB), 65 μm PDMS/DVB, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 3, pink hub
Supelco
Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 3, light blue hub
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Gruppo fibre SPME poliacrilato (PA), 85 μm Polyacrylate, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, white hub
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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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SPME Portable Field Sampler, coating PDMS/DVB
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Gruppo fibre SPME polidimetilsilossano/divinilbenzene (PDMS/DVB), 65 μm PDMS/DVB, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, pink hub
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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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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, light blue hub
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Gruppo fibre SPME poliacrilato (PA), 85 μm Polyacrylate, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, white hub
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Gruppo fibre SPME polidimetilsilossano/divinilbenzene (PDMS/DVB), 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, blue hub
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SPME Portable Field Sampler, coating PDMS
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SPME Fiber Assembly Kit, Assortment, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 4
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Gruppo in fibra SPME carbossene/polidimetilsilossano (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, black hub
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Unità fibra SPME polidimetilsilossano (PDMS), 100 μm PDMS, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, red hub
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SPME Fiber Assembly Kit, Assortment, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 4
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SPME Portable Field Sampler, coating CAR/PDMS