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  • Solid-phase microextraction for the determination of haloanisoles in wines and other alcoholic beverages using gas chromatography and atomic emission detection.

Solid-phase microextraction for the determination of haloanisoles in wines and other alcoholic beverages using gas chromatography and atomic emission detection.

Journal of chromatography. A (2008-10-18)
Natalia Campillo, Rosa Peñalver, Manuel Hernández-Córdoba
ABSTRACT

A headspace solid-phase microextraction (HS-SPME) method for the determination of 12 haloanisoles in wine and spirit samples using gas chromatography with atomic emission detection (GC-AED) was developed. The different factors affecting the efficiency of the extraction were carefully optimized. The divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was the most suitable for preconcentrating the analytes from the headspace of the sample solution. water dilutions of 3:4 and 1:6 for wines and spirits, respectively, and the use of a mixed bromochloroanisole compound as internal standard allowed sample quantification against external standards prepared in the presence of 5% (v/v) ethanol. Detection limits ranged from 1.2 to 18.5ngL(-1), depending on the compound and the sample analyzed, with a fiber time exposure of 60min at 75 degrees C. The optimized method was successfully applied to different samples, and several of the studied haloanisoles were detected at concentration levels ranging from 10.3ngL(-1) to 1.14ngmL(-1).

MATERIALS
Product Number
Brand
Product Description

Supelco
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
Supelco
Carboxen® 569, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
Sigma-Aldrich
2-Chloroanisole, 98%
Supelco
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)
Supelco
ORBO 78 HBr on Carboxen® 564 specially cleaned (20/45), 400/200 mg, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
Supelco
Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler