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

161438

Sigma-Aldrich

2-Chloroanisole, 98%

20358

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)

20355

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

29534-U

Supelco

Carboxen^® 569, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea

28718-U

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

11324-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 564, 20-45 mesh, pack of 144 × 290 mg

24241-U

Supelco

Carboxen^®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm

25461

Supelco

Carboxen^®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm

24246

Supelco

Carboxen^®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm

25467

Supelco

Carboxen^®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm

10471

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1003, 40-60 mesh, bottle of 10 g

10478-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1000, 60-80 mesh, bottle of 10 g

57298-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler

57344-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder

10477-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 1000, 40-60 mesh, bottle of 50 g

57328-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder

57335-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler

57299-U

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

57295-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler

57348-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex

57329-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler

57343-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler

57318

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga

57334-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber

57319

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler

10269

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 569, 20-45 mesh, bottle of 10 g

57906-U

Supelco

SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), d_f 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber

57914-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm

57912-U

Supelco

SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm

11072-U

Supelco

Carboxen^® Adsorbent, matrix Carboxen^® 572, 20-45 mesh, bottle of 10 g