title: Monolithic spin column: a new extraction device for analysis of drugs in urine and serum by GC/MS and HPLC/MS.
abstract: A monolithic spin column was developed for the extraction of analytes from biological materials. This column was constructed by packing a monolithic silica disk into a spin column. Sample loading, washing, and elution of the target drugs were accomplished simply by centrifugation of the column. Opiates and benzodiazepines are abused throughout the world. Identification and quantification of these drugs is very important to solve crimes or the cause of death. Three opiates (morphine, codeine, and dihydrocodeine) were extracted from urine and serum by using the column. After conversion to trimethylsilyl derivatives of the opiates by vigorous mixing with the derivatizing reagent, the solution was subjected to GC/MS. A linear curve was observed for opiates from 10 to 2500 ng/mL in urine and 5 to 1200 ng/mL in serum, respectively (correlation coefficient > 0.996). For benzodiazepines, the hydroxyl metabolites of triazolam and etizolam were extracted from urine using the column, and the eluate was directly analyzed by HPLC/MS without evaporation. The LOD values were at the ppb level, with RSD values lower than 15%. The proposed methods were successfully applied to clinical and forensic cases, and good agreement of results was obtained compared to conventional methods.
authors.affiliation: Hiroshima University, Graduate School of Biomedical Sciences, Department of Forensic Medicine, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551, Japan. namera@hiroshima-u.ac.jp
authors.forename: Akira
authors.initials: A
authors.lastname: Namera
authors.forename: Masakata
authors.initials: M
authors.lastname: Nagao
authors.forename: Akihiro
authors.initials: A
authors.lastname: Nakamoto
authors.forename: Shota
authors.initials: S
authors.lastname: Miyazaki
authors.forename: Takeshi
authors.initials: T
authors.lastname: Saito
mesh_terms: D000701:Analgesics, Opioid / Q000737:chemistry; D001569:Benzodiazepines / Q000737:chemistry; D001774:Blood Chemical Analysis / Q000379:methods*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D015394:Molecular Structure; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D014556:Urine / Q000737:chemistry*
chemical_list: D000701:Analgesics, Opioid; D001569:Benzodiazepines