Rapid derivatization of phosphorus-containing amino acid herbicides in plasma and urine using microwave heating.

We developed a derivatization technique that involves microwave heating to reduce the overall forensic analysis time of phosphorus-containing amino acid herbicides (PAAHs). Combined with an extraction method that uses titanium (IV) oxide (TiO2), we were able to obtain a practical analytical method for PAAHs and their metabolites in samples intended for poisoning cases. The optimized derivatization conditions were 700 W power and 5-min irradiation time, which is a significant time-saving. The plasma samples extracted using TiO2-packed Tip columns and derivatized under the optimized conditions had an intra-day accuracy and precision within 9.3% and 9.0%, respectively. The intermediate accuracy and precision were within 8.8% and 8.5%, respectively, and the recoveries were more than 91.2%. Similarly, for urine samples, the intra-day accuracy and precision were within 13.3% and 9.1%, respectively. The intermediate accuracy and precision were within 13.6% and 10.3%, respectively, and finally, the recoveries were more than 88.2%. In addition to reducing the pretreatment time, this method was suitable for reducing the overall labor burden on laboratories responsible for routine analysis because of its stable validation data.

Analysis of hallucinogenic constituents in Amanita mushrooms circulated in Japan.

The constituents of seven mushrooms sold as Amanita muscaria or Amanita pantherina (five A. muscaria and two A. pantherina) and four "extracts purported to contain A. muscaria" products that are currently circulated in Japan were determined. All mushroom samples were identified as A. muscaria or A. pantherina by macroscopic and microscopic observation. The dissociative constituents, ibotenic acid (IBO) and muscimol (MUS), were extracted with 70% methanol twice and determined by gas chromatography/mass spectrometry. The IBO (as the hydrate)/MUS contents were in the range of <10-2845ppm/46-1052ppm in the cap of A. muscaria and 188-269ppm/1554-1880ppm in the cap of A. pantherina. In the caps, these compounds had a tendency to be more concentrated in the flesh than in the cuticle. On the other hand, the IBO/MUS contents in the stem were far lower than in the caps. In the "extracts purported to contain A. muscaria" products, IBO/MUS were detected below the lower limit of calibration curve (<10ppm/<25ppm) or not detected. However, these samples contained other psychoactive compounds, such as psychoactive tryptamines (5-methoxy-N,N-diisopropyltryptamine and 5-methoxy-N,N-dimethyltryptamine), reversible monoamine oxidase inhibitors (harmine and harmaline) and tropane alkaloids (atropine and scopolamine), which were not quantified. This is the first report of the chemical analysis of Amanita mushrooms that are circulated in the drug market.