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  • Analysis of volatile contaminants in vegetable oils by headspace solid-phase microextraction with carboxen-based fibres.

Analysis of volatile contaminants in vegetable oils by headspace solid-phase microextraction with carboxen-based fibres.

Journal of chromatography. A (2000-04-11)
B D Page, G Lacroix
ABSTRACT

The headspace solid-phase microextraction (HS-SPME) efficiencies from vegetable oil of the recently available Carboxen-poly(dimethylsiloxane) (PDMS) and divinylbenzene-Carboxen-PDMS fibres were found to be much greater than those of the PDMS fibre for a number of volatile contaminants. Using these Carboxen-based fibres, the commonly used HS-SPME equilibration times for aqueous matrices of 30-45 min at room temperature for a number of halogenated and aromatic analytes with volatilities ranging from 1,1-dichloroethylene to hexachlorobenzene were found to be insufficient for the effective extraction of the less volatile analytes from vegetable oil. HS-SPME at 100 degrees C for 45 min, followed by rapid cooling to 0 degrees C with a 10 min continuing extraction, however, significantly increased the SPME efficiencies for the less volatile analytes. Spiking solutions were prepared in vegetable oil instead of methanol as the latter was found to displace analytes from the Carboxen material. Using either of the Carboxen-based fibres and SPME at 100 degrees C, all the target analytes could be determined at low or sub-microg kg(-1) with repeatability < or =10%, even though an equilibrium SPME of the less volatile analytes was not achieved.

MATERIALS
Product Number
Brand
Product Description

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
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
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
Graphsphere Adsorbent, matrix Graphsphere 2016, 60-80 mesh, bottle of 10 g
Supelco
Carboxen® 569, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
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
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 Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler
Supelco
Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, pack of 144 × 290 mg
Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
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 24 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 autosampler
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
Supelco
Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
Supelco
Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
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, for use with autosampler, needle size 23 ga, metal alloy fiber
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
Supelco
Carboxen® Adsorbent, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g