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  • Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2002-05-23)
Frank Sporkert, Fritz Pragst, Sandra Hübner, Graham Mills
PMID12016014
ABSTRACT

A new and in part automated headspace solid-phase microextraction method for quantitative determination of the highly toxic rodenticide fluoroacetic acid (FAA) in serum and other biological samples has been developed. FAA and deuterated acetic acid (internal standard) were extracted from acidified samples by a StableFlex divinylbenzene-Carboxen on polydimethylsiloxane fibre. The acids were derivatised on the fibre in-situ with 1-pyrenyldiazomethane and detected using gas chromatography-mass spectrometry with electron impact ionisation and selected ion monitoring. The calibration curve for FAA in serum was linear over the range from 0.02 to 5 microg/ml, with limits of detection and quantification of 0.02 and 0.07 microg/ml, respectively. The method was also tested with spiked whole blood, urine, stomach contents and kidney samples. It was sufficiently reliable, reproducible and sensitive for use in routine forensic toxicology applications.

MATERIALS
Product Number
Brand
Product Description
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
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57906-U
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SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, for use with autosampler, needle size 23 ga, metal alloy fiber
57914-U
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SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm
54041-U
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Carboxen® 1000 Reversible SPE Tube, 200 mg/mL, pk 30
11048-U
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Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g
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
P6863
Sigma-Aldrich
PDAM, for HPLC derivatization
57298-U
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler
57295-U
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
57343-U
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
10477-U
Supelco
Carboxen® Adsorbent, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
57335-U
Supelco
SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
57328-U
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, for use with manual holder
10478-U
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25467
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Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
10269
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Carboxen® Adsorbent, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
57348-U
Supelco
SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex
24246
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Carboxen®-1010 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
25461
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Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
10263
Supelco
Carboxen® Adsorbent, matrix Carboxen® 563, 20-45 mesh, bottle of 10 g
10264
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Carboxen® Adsorbent, matrix Carboxen® 564, 20-45 mesh, bottle of 10 g
10471
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Carboxen® Adsorbent, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
57318
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SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
57334-U
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SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
57319
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SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
57329-U
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SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 24 ga, StableFlex, for use with autosampler
57344-U
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SPME fiber assembly Carboxen/Polydimethylsiloxane (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
24241-U
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Carboxen®-1006 PLOT Capillary GC Column, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
23446-U
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ORBO™-93 Sorbent Tube, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea