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CN
  • 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
摘要

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.

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Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 24 ga, Autosampler, pk of 3, notched gray hub
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Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1cm), needle size 24 ga, Manual Holder, pk of 3, plain gray hub
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Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 23 ga, Autosampler, pk of 3, plain gray hub
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Supelco
ORBO Carboxen-564 管, W,F,F separators, O.D. × L 6 mm × 75 mm, pkg of 25 ea, for analyte group MEK (methylethyl ketone)
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Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, plain gray hub
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Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, StableFlex (2cm), needle size 23 ga, Autosampler, pk of 3, notched gray hub
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Supelco
ORBO-78 400/200mg,每包 25 支, W,W,W separators, O.D. × L 6 mm × 110 mm, pkg of 25 ea
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Supelco
Carboxen®1010 多孔层壁涂开管柱, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 75 μm(CAR/PDMS, for use with manual holder, needle size 24 ga
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Supelco
Carbopack®吸附剂, matrix Carboxen® 1000, 60-80 mesh, bottle of 10 g
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Supelco
Carboxen® 1006 多孔层壁涂开管柱, L × I.D. 30 m × 0.53 mm, average thickness 30 μm
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Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 23 ga, StableFlex, for use with autosampler
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Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, StableFlex, for use with autosampler
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Supelco
Carboxen®1010 多孔层壁涂开管柱, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 24 ga, for use with autosampler
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Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 85 μm(CAR/PDMS, needle size 24 ga, for use with manual holder, StableFlex fiber
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Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with autosampler
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Supelco
SPME固相微萃取萃取头 Carboxen/聚二甲基硅氧烷 (CAR/PDMS), df 75 μm(CAR/PDMS, needle size 23 ga, for use with manual holder
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Supelco
Carboxen® 1006 多孔层壁涂开管柱, L × I.D. 30 m × 0.32 mm, average thickness 15 μm
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Supelco
Carboxen® 1000 双向固相萃取管, 200 mg/mL, pk 30
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Supelco
Carbopack®吸附剂, matrix Carboxen® 572, 20-45 mesh, bottle of 10 g
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Supelco
Carbopack®吸附剂, matrix Carboxen® 1000, 40-60 mesh, bottle of 50 g
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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
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Supelco
Carbopack®吸附剂, matrix Carboxen® 569, 20-45 mesh, bottle of 10 g
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Carbopack®吸附剂, matrix Carboxen® 1003, 40-60 mesh, bottle of 10 g
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Supelco
ORBO-93吸附管, ORBO tube I.D. × L 6 mm × 95 mm, Bed A 180 mg, Bed B 90 mg, 60/80 mesh, pkg of 25 ea
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Supelco
SPME 纤维组件二乙烯基苯/羧基/聚二甲基硅氧烷 (DVB/CAR/PDMS), 50/30µm DVB/CAR/PDMS, Metal Alloy (1cm), needle size 23 ga, Autosampler, pk of 1 ×, plain gray hub
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Supelco
Carbopack®吸附剂, matrix Carboxen® 569, 20-45 mesh, bottle of 500 g
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Supelco
Carboxen® 572 for Tobacco Smoke, Adsorbent Bed Wt: 300 mg, cartridge size 3 mL, pkg of 50 ea
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Carboxen® 569, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
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