A fully automated procedure using alkaline hydrolysis and headspace solid-phase microextraction (HS-SPME), followed by on-fiber derivatization and gas chromatographic-mass spectrometric (GC-MS) detection has been developed for determination of cannabinoids in hemp food samples. After addition of a deuterated internal standard, the sample was hydrolyzed with sodium hydroxide and submitted to direct HS-SPME. After absorption of analytes for on-fiber derivatization, the fiber was placed directly into the headspace of a second vial containing N-methyl- N-trimethylsilyltrifluoroacetamide (MSTFA), before GC-MS analysis.
View Article and Find Full Text PDFFour commonly used immunoassay kits were evaluated for their efficiency in screening for drugs of abuse in whole blood. Six groups of illicit drugs (opiates, cannabinoids, amphetamines, cocain and benzoylecgonine, benzodiazepines, and methadone) were determined by using the homogenous assays ADx and CEDIA DAU and compared with the results produced by means of the inhomogenous assays MTP and Pyxis 24. The measured 86 blood samples were taken from authentic routine analyses between February and September, 2000.
View Article and Find Full Text PDFThis article describes a fully automated procedure for detecting cannabinoids in human hair samples. The procedure uses alkaline hydrolysis and headspace solid-phase dynamic extraction (HS-SPDE), followed by on-coating derivatization and gas chromatography-mass spectrometry (GC-MS). SPDE is a further development of solid-phase microextraction (SPME), based on an inside needle capillary absorption trap.
View Article and Find Full Text PDFA new method combination, headspace solid-phase dynamic extraction coupled with gas chromatography/tandem mass spectrometry (HS-SPDE/GC/MS/MS), is introduced to determine drugs of abuse in hair samples. This highly automated procedure utilizes SPDE for pre-concentration and on-coating derivatization as well as GC and triple quadrupole MS/MS for selective and sensitive detection. All these steps, apart from washing and cutting of the hair samples, are performed without manual intervention on a robot-like autosampler.
View Article and Find Full Text PDFThis paper describes a fully automated procedure using alkaline hydrolysis and headspace solid-phase microextraction (HS-SPME) followed by on-fiber derivatization and gas chromatographic-mass spectrometric (GC-MS) detection of cannabinoids in human hair samples. Ten milligrams of hair was washed with deionized water, petroleum ether, and dichloromethane. After the addition of deuterated internal standards the sample was hydrolyzed with sodium hydroxide and directly submitted to HS-SPME.
View Article and Find Full Text PDFThis study describes a fully automated procedure using alkaline hydrolysis and headspace (HS) solid-phase microextraction (SPME) followed by on-fiber derivatization and gas chromatographic (GC)-mass spectrometric (MS) detection of amphetamine, methamphetamine, methylendioxyamphetamine, methylendioxymethamphetamine, methylendioxyethylamphetamine, methylendioxyphenylbutanamine, and methylmethylendioxyphenylbutanamine in human hair samples. Ten milligrams of hair is washed with deionized water, petroleum ether, and dichloromethane. After the addition of deuterated internal standards the sample is hydrolyzed with sodium hydroxide and directly submitted to HS-SPME.
View Article and Find Full Text PDFThe technique of automated headspace solid-phase dynamic extraction (SPDE) coupled with gas chromatography-mass spectrometry was evaluated for the determination of amphetamines and synthetic designer drugs in hair samples. Headspace SPDE is a novel method for the solventless extraction of organic compounds in aqueous samples. In a so-called inside needle capillary absorption trap a hollow needle with an internal coating of polydimethylsiloxane is used as extraction and preconcentration medium.
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