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Screening for 2-acetyl-1-pyrroline in the headspace of rice using SPME/GC-MS.

Journal of agricultural and food chemistry (2001-02-15)
C C Grimm, C Bergman, J T Delgado, R Bryant
ZUSAMMENFASSUNG

Solid phase microextraction (SPME) is used to collect and concentrate the compounds in the headspace of rice. This research describes optimization parameters of temperature, moisture, and sampling time. Optimization was based upon the recovered levels of 2-acetyl-1-pyrroline (2-AP), the popcorn aroma in aromatic rice. The method uses a sampling temperature of 80 degrees C and adds 100 microL of water to a 0.75 g sample of rice. The rice was preheated for 25 min, a carboxen/DVB/PDMS SPME fiber was exposed to the headspace for 15 min, and a subsequent GC-MS analysis took 35 min. Samples of rice can be analyzed as the flour, milled kernels, or brown rice. Twenty-one experimental rice varieties were analyzed by the SPME method and compared to a wet technique. Recoveries of several nanograms of 2-AP from 0.75 g samples of aromatic rice were observed, whereas only trace amounts of 2-AP were recovered from nonaromatic rice. Recovery from a single SPME headspace analysis is calculated to be 0.3% of the total 2-AP in the sample.

MATERIALIEN
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Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub
Supelco
ORBO Carboxen-564 Röhrchen, 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 auf Carboxen® 564 speziell gereinigt (20/45), 400/200 mg, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
Supelco
Carboxen®-1010 PLOT Kapillar-GC-Säule, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, black hub
Supelco
Carboxen®-1006 PLOT Kapillar-GC-Säule, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, black hub
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, light blue hub
Supelco
Carboxen®-1010 PLOT Kapillar-GC-Säule, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Manual Holder, pk of 3, light blue hub
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, light blue hub
Supelco
ORBO-93 Sorbensröhrchen, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Autosampler, pk of 3, black hub
Supelco
Carboxen®-1006 PLOT Kapillar-GC-Säule, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 75 μm CAR/PDMS, Fused Silica (1 cm), needle size 23 ga, Manual Holder, pk of 3, black hub
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, Metal Alloy (2cm), needle size 23 ga, Autosampler, pk of 1, plain gray hub
Supelco
Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea
Supelco
SPME-Faseranordnung, 50/30µm DVB/CAR/PDMS, Metal Alloy (1cm), needle size 23 ga, Autosampler, pk of, plain gray hub
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
Supelco
Carboxen® 1000 Reversibles SPE-Röhrchen, 200 mg/mL, pk 30
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
Supelco
Carboxen® Adsorptionsmittel, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
Supelco
SPME-Faseranordnung Carboxen/Polydimethylsiloxan (CAR/PDMS), 85 μm CAR/PDMS, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, light blue hub