Pesticide residues analysis in cannabis: optimization of clean-up strategy and comparison of GC-MS/MS and GCxGC-MS techniques potential

Kód výsledku v IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F60461373%3A22330%2F22%3A43925444" target="_blank" >RIV/60461373:22330/22:43925444 - isvavai.cz</a>

Výsledek na webu

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DOI - Digital Object Identifier

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Jazyk výsledku

angličtina

Název v původním jazyce

Pesticide residues analysis in cannabis: optimization of clean-up strategy and comparison of GC-MS/MS and GCxGC-MS techniques potential

Popis výsledku v původním jazyce

Determination of pesticide residues in such complex matrix as Cannabis is a challenging task, as the plant contains number of components including phytocannabinoids, terpenes, phenolic substances, that are co-extracted and impair accurate analysis. Due to a high ´chemical noise´, achieving low LOQs and other performance characteristics for some pesticides is rather difficult. In this study, we focused on selection of the most effective clean-up strategy for purification of QuEChERS extract obtained by extraction of matrix spiked by 288 GC-amenable pesticides (x mg/kg). Following approaches were tested (i) dispersive solid phase extraction (dSPE) by primary - secondary amine (PSA), (ii) freezing out followed by dSPE using PSA, (iii) dSPE using Chlorofiltr sorbent (from UCT), (iv) dSPE using Supel QuE-Verde (Supelco), (v) dSPE using mixture of PSA, Bondesil-C18 and EnviCarb, (vi) solid phase extraction by PSA cartridge (from UCT, 1 and 3 mL of extract), (vii) SPE (PSA cartridge) followed by dSPE by PSA. In the first phase GC-MS/MS (Agilent 7890B gas chromatograph coupled with Agilent 7010 GC-TQ mass spectrometer was used). Obtained data were critically assessed against criteria defined in SANTE/11312/2021 document. The best results were obtained by Supel Que-Verde sorbent clean-up with the highest number of pesticide residues, which performance characteristics met the required parameters. In the second part of study, GCxGC-MS technique (employing Agilent 7890B gas chromatograph coupled with LECO BT 4D TOF mass spectrometer) was used for analyses in order to separate, at least partly co-extracts still remaining in purified extract and improve detectability. When comparing the investigated techniques, the results showed that higher number of pesticides (85 %) was detected by GC-MS/MS compared to GCxGC-MS (55 %), on the other hand, the latter technique enabled to detect some of the pesticides e.g. carboxin or desmedipham, problematic in GC-MS/MS.

Název v anglickém jazyce

Pesticide residues analysis in cannabis: optimization of clean-up strategy and comparison of GC-MS/MS and GCxGC-MS techniques potential

Popis výsledku anglicky

Determination of pesticide residues in such complex matrix as Cannabis is a challenging task, as the plant contains number of components including phytocannabinoids, terpenes, phenolic substances, that are co-extracted and impair accurate analysis. Due to a high ´chemical noise´, achieving low LOQs and other performance characteristics for some pesticides is rather difficult. In this study, we focused on selection of the most effective clean-up strategy for purification of QuEChERS extract obtained by extraction of matrix spiked by 288 GC-amenable pesticides (x mg/kg). Following approaches were tested (i) dispersive solid phase extraction (dSPE) by primary - secondary amine (PSA), (ii) freezing out followed by dSPE using PSA, (iii) dSPE using Chlorofiltr sorbent (from UCT), (iv) dSPE using Supel QuE-Verde (Supelco), (v) dSPE using mixture of PSA, Bondesil-C18 and EnviCarb, (vi) solid phase extraction by PSA cartridge (from UCT, 1 and 3 mL of extract), (vii) SPE (PSA cartridge) followed by dSPE by PSA. In the first phase GC-MS/MS (Agilent 7890B gas chromatograph coupled with Agilent 7010 GC-TQ mass spectrometer was used). Obtained data were critically assessed against criteria defined in SANTE/11312/2021 document. The best results were obtained by Supel Que-Verde sorbent clean-up with the highest number of pesticide residues, which performance characteristics met the required parameters. In the second part of study, GCxGC-MS technique (employing Agilent 7890B gas chromatograph coupled with LECO BT 4D TOF mass spectrometer) was used for analyses in order to separate, at least partly co-extracts still remaining in purified extract and improve detectability. When comparing the investigated techniques, the results showed that higher number of pesticides (85 %) was detected by GC-MS/MS compared to GCxGC-MS (55 %), on the other hand, the latter technique enabled to detect some of the pesticides e.g. carboxin or desmedipham, problematic in GC-MS/MS.

Druh

O - Ostatní výsledky

CEP obor

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OECD FORD obor

10406 - Analytical chemistry

Projekt

<a href="/cs/project/LM2018100" target="_blank" >LM2018100: Infrastruktura pro propagaci metrologie v potravinářství a výživě v České republice</a><br>

Návaznosti

P - Projekt vyzkumu a vyvoje financovany z verejnych zdroju (s odkazem do CEP)

Rok uplatnění

2022

Kód důvěrnosti údajů

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů