Fast extraction of cannabinoids in marijuana samples by using hard-cap espresso machines.

A simple, quick and low cost procedure was developed for the extraction of Δ9-tetrahydrocannabinol, cannabidiol, and cannabinol from marijuana samples, based on the use of a hard-cap espresso extraction with 2-propanol. After extraction, cannabinoids were directly determined after appropriate dilution by gas-chromatography-mass spectrometry, reaching a limit of detection from 0.03 to 0.05 mg g-1. Extraction efficiency was evaluated by the comparison of results obtained for seized samples by the proposed method and a reference methodology based on ultrasound-assisted extraction. Moreover, ion mobility was proposed for the rapid and sensitive determination of Δ9-tetrahydrocannabinol and cannabidiol providing a quick response for the analysis of seized marijuana samples in 1 min, including extraction, dilution and determination.

Identification and determination of synthetic cannabinoids in herbal products by dry film attenuated total reflectance-infrared spectroscopy.

A new procedure has been developed for the identification and quantitative determination of synthetic cannabinoids in illicit herbal preparations. The methodology is based on the use of attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) measurement of sample extracts with 2-propanol drying 5µL of the extracts onto the ATR crystal. The qualitative identification was carried out on the 2-propanol extract after identification of the herbal matrix, followed by its subtraction and using a cut-off criterion of 75%. Quantitative determination was made by univariate calibration using the absorbance of the band located at 1520cm-1 of the spectrum. Four different cannabinoids, RCS-4, JWH-210, UR-144 and JWH-081 were used as test analytes and the ATR-FTIR method provided limits of quantification from 14 till 79mgL-1. Sized blank market samples were successfully identified and UR-144 quantified.

Ion mobility spectrometry for monitoring diamine oxidase activity.

The capability of IMS for the determination of kinetics in complex enzyme systems with reduced v(max) values has been demonstrated with the example of diamine oxidase (DAO). Michaelis-Menten and Lineweaver-Burk plots were obtained for the enzyme catalyzed putrescine oxidation and calculations of the kinetic parameters have been performed and compared with previously published values. The IMS procedure provided a limit of detection of 200 pg mL(-1) for putrescine, a limit of quantification of 667 pg mL(-1), a precision of 5.9%, and an analysis frequency of 40 s, which are analytical characteristics appropriate to perform label-free enzyme studies. Additionally, pseudo-competitive inhibition of the putrescine oxidation due to other diamines binding to the free enzyme has been evaluated. Moreover, the mass-mobility correlation curve of diamines based on the calculated mobilities of the studied analytes and data previously reported for cadaverine, serotonin and tryptamine was modelled. The analytical method could be used as an additional complementary tool for the existing drug discovery method, for the search of DAO activators; molecules that displace the substrate from the second site of DAO, but does not interfere with the catalytic function of the first site.