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

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

20355

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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

20358

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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)

57906-U

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

11072-U

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

11048-U

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Carboxen^® Adsorbent, matrix Carboxen^® 569, 20-45 mesh, bottle of 500 g

54041-U

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Carboxen^® 1000 Reversible SPE Tube, 200 mg/mL, pk 30

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

10477-U

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

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

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

10478-U

Supelco

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

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

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

57328-U

Supelco

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

57329-U

Supelco

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

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

57343-U

Supelco

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

P6863

Sigma-Aldrich

PDAM, for HPLC derivatization

24246

Supelco

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

10471

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

25461

Supelco

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