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

RESUMEN

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.

MATERIALES

Referencia del producto

Marca

Descripción del producto

57348-U

Supelco

Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, StableFlex

57328-U

Supelco

Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, for use with manual holder

57298-U

Supelco

Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 23 ga, StableFlex, for use with autosampler

57299-U

Supelco

Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm

57329-U

Supelco

Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, needle size 24 ga, StableFlex, for use with autosampler

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-78 400/200 MG PK/25, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea

10478-U

Supelco

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

25467

Supelco

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

57318

Supelco

Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, d_f 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga

57295-U

Supelco

Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, d_f 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler

25461

Supelco

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

57319

Supelco

Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, d_f 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler

57335-U

Supelco

Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, d_f 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler

24246

Supelco

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

57334-U

Supelco

Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, d_f 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber

57343-U

Supelco

Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, d_f 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler

57344-U

Supelco

Fibra de carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, d_f 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder

11072-U

Supelco

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

24241-U

Supelco

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

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

10477-U

Supelco

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

10269

Supelco

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

10471

Supelco

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

57914-U

Supelco

Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 2 cm

54041-U

Supelco

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

23446-U

Supelco

Tubo absorbente ORBO^™-93, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea

57912-U

Supelco

Fibra de divinilbenceno/carboxeno/polidimetilsiloxano (DVB/CAR/PDMS) de SPME, for use with autosampler, needle size 23 ga, metal alloy fiber, fiber L 1 cm

P6863

Sigma-Aldrich

PDAM, for HPLC derivatization

11048-U

Supelco

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