Solvent-modified solid-phase microextraction for the determination of diazepam in human plasma samples by capillary gas chromatography

• Published in: Journal of chromatography. B, Biomedical sciences and applications Biomedical sciences and applications, 1997-02, Vol.689 (2), p.357-364
• Main Authors: Krogh, Mette, Grefslie, Hege, Rasmussen, Knut E.
• Format: Article
• Language: English
• Subjects: Acetic Acid - chemistry; Analysis; Biological and medical sciences; Chromatography, Gas - methods; Diazepam; Diazepam - blood; Diazepam - isolation & purification; General pharmacology; Humans; Ketones - chemistry; Medical sciences; Pharmacology. Drug treatments; Solvents - chemistry
• ISSN: 0378-4347; 1387-2273
• DOI: 10.1016/S0378-4347(96)00352-0

This paper describes microextraction and gas chromatographic analysis of diazepam from human plasma. The method was based on immobilisation of 1.5 μl of 1-octanol on a polyacrylate-coated fiber designed for solid-phase microextraction. The solvent-modified fibre was used to extract diazepam from the samples. The plasma sample was pre-treated to release diazepam from the protein binding. The fibre was inserted into the modified plasma sample, adjusted to pH 5.5, an internal standard was added and the mixture was carefully stirred for 4 min. The fibre with the immobilised solvent and the enriched analytes was injected into the capillary gas chromatograph. The solvent and the extracted analytes were evaporated at 300°C in the split-splitless injection port of the gas chromatograph, separated on a methylsilicon capillary column and detected with a nitrogen-phosphorus detector. The method was shown to be reproducible with a detection limit of 0.10 nmol/ml in human plasma.