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Direct screening of herbal blends for new synthetic cannabinoids by MALDI-TOF MS.

Journal of mass spectrometry : JMS (2012-01-28)
Rossella Gottardo, Anna Chiarini, Ilaria Dal Prà, Catia Seri, Claudia Rimondo, Giovanni Serpelloni, Ubaldo Armato, Franco Tagliaro
ABSTRACT

Since 2004, a number of herbal blends containing different synthetic compounds mimicking the pharmacological activity of cannabinoids and displaying a high toxicological potential have appeared in the market. Their availability is mainly based on the so-called "e-commerce", being sold as legal alternatives to cannabis and cannabis derivatives. Although highly selective, sensitive, accurate, and quantitative methods based on GC-MS and LC-MS are available, they lack simplicity, rapidity, versatility and throughput, which are required for product monitoring. In this context, matrix-assisted laser desorption ionization-time of flight mass spectrometry (MALDI-TOF MS) offers a simple and rapid operation with high throughput. Thus, the aim of the present work was to develop a MALDI-TOF MS method for the rapid qualitative direct analysis of herbal blend preparations for synthetic cannabinoids to be used as front screening of confiscated clandestine preparations. The sample preparation was limited to herbal blend leaves finely grinding in a mortar and loading onto the MALDI plate followed by addition of 2 µl of the matrix/surfactant mixture [α-cyano-4-hydroxy-cinnamic acid/cetyltrimethylammonium bromide (CTAB)]. After drying, the sample plate was introduced into the ion source for analysis. MALDI-TOF conditions were as follows: mass spectra were analyzed in the range m/z 150-550 by averaging the data from 50 laser shots and using an accelerating voltage of 20 kV. The described method was successfully applied to the screening of 31 commercial herbal blends, previously analyzed by GC-MS. Among the samples analyzed, 21 contained synthetic cannabinoids (namely JWH-018, JWH-073, JWH-081, JWH-250, JWH-210, JWH-019, and AM-694). All the results were in agreement with GC-MS, which was used as the reference technique.

MATERIALS
Product Number
Brand
Product Description

Supelco
α-Cyano-4-hydroxycinnamic acid, matrix substance for MALDI-MS, ≥99.0% (HPLC)
Sigma-Aldrich
α-Cyano-4-hydroxycinnamic acid, suitable for MALDI-TOF MS
Sigma-Aldrich
α-Cyano-4-hydroxycinnamic acid, ≥98% (TLC), powder
Sigma-Aldrich
α-Cyano-4-hydroxycinnamic acid, matrix substance for MALDI-MS, Ultra pure
Sigma-Aldrich
α-Cyano-4-hydroxycinnamic acid, 99%
Sigma-Aldrich
α-Cyano-4-hydroxycinnamic acid, 97%

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