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  • Determination of volatile oak compounds in wine by headspace solid-phase microextraction and gas chromatography-mass spectrometry.

Determination of volatile oak compounds in wine by headspace solid-phase microextraction and gas chromatography-mass spectrometry.

Journal of chromatography. A (2005-11-11)
José David Carrillo, Alvaro Garrido-López, María Teresa Tena
RESUMEN

A headspace solid-phase microextraction (HS-SPME) and gas chromatography (GC) coupled to mass spectrometry (MS) method was developed to identify and quantify 14 volatile oak compounds in aged red wines. The most important HS-SPME variables were optimised by experimental design technique in order to improved the extraction process. The selected conditions were: 10 mL of sample in 20 mL sealed vials with addition of 30% of sodium chloride (saturated solution), divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) fibre, 10 min of pre-incubation time, 70 degrees C of temperature and 60 min of extraction time without agitation. The features of the method were established for the studied compounds in terms of linear range, slope and intercept of the calibration graphs, detection and quantification limits and repeatability. For all compounds detection limits were below their threshold levels and repeatability, in terms of relative standard deviation, was good, with values between 3 and 11%. Finally, the method was applied to the analysis of six aged red wines by both internal standard and standard addition calibration methods. The concentrations obtained with both methods were statistically compared.

MATERIALES
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Supelco
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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ORBO 90 Carboxen® 564 (20/45) 160/80 mg, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)
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Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
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ORBO-78 400/200 MG PK/25, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
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Columna capilar para GC Carboxen®-1010 PLOT, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
Supelco
Columna capilar para GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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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
Supelco
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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Columna capilar para GC Carboxen®-1010 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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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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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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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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Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
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Columna capilar para GC Carboxen®-1006 PLOT, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Tenax® TA / Carboxen® 1018, glass TD tube, preconditioned, O.D. × L 1/4 in. × 3 1/2 in., Sealed with (Swagelok® End-Fittings), pkg of 10 ea
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Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
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Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
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Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
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Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
Sigma-Aldrich
γ-Nonanoic lactone, 97%
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Tubo absorbente ORBO-93, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea
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Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm
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Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g