Several molecularly imprinted polymers (MIPs) have been synthesized for the first time using various synthetic cannabinoids (JWH007, JWH015 and JWH098) as template molecules. Ethylene dimethacrylate (EDMA) was used as a functional monomer for all cases. Similarly, divinylbenzene (DVB) and 2,2′-azobisisobutyronitrile (AIBN) were used as cross-linker and initiator, respectively. The prepared MIPs have been fully characterized and evaluated as new selective adsorbents for micro-solid phase extraction (μ-SPE) of synthetic cannabinoids in urine. The developed MIP-μ-SPE devices consisted of a polypropylene (PP) porous membrane containing the adsorbent (novel porous membrane protected micro-solid phase extraction based on a cone-shaped device) for operating in batch mode, which allowed a fast and integrated extraction-cleanup procedure. High performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) was used for quantifying the analytes after MIP-μ-SPE. The best performances were obtained for MIPs prepared from JWH015 as a template. Optimum loading conditions were found to be urine pH of 5.0 and adsorption time of 8.0 min under mechanical (orbital-horizontal) stirring at 100 rpm. The composition of the eluting solution consisted of 75:20:5 heptane/2-propanol/ammonium hydroxide. The elution was assisted by ultrasounds (37 kHz, 325 W) for 8.0 min. In addition, studies regarding selectivity have also been addressed for several drugs of abuse under optimized loading/adsorption conditions. Validation of the method showed good precision and analytical recovery by intra-day and inter-day assays (RSD values lower than 7 and 10% for intra-day and inter-day precision, and within the 83–100% range for intra-day and inter-day analytical recovery).

Sánchez-González, J., Odoardi, S., Bermejo, A. M., Bermejo-Barrera, P., Romolo, F. S., Moreda-Piñeiro, A., Strano Rossi, S., Development of a micro-solid-phase extraction molecularly imprinted polymer technique for synthetic cannabinoids assessment in urine followed by liquid chromatography–tandem mass spectrometry, <<JOURNAL OF CHROMATOGRAPHY A>>, 2018; 1550 (n/a): 8-20. [doi:10.1016/j.chroma.2018.03.049] [http://hdl.handle.net/10807/119455]

Development of a micro-solid-phase extraction molecularly imprinted polymer technique for synthetic cannabinoids assessment in urine followed by liquid chromatography–tandem mass spectrometry

Odoardi, Sara
Membro del Collaboration Group
;
Romolo, Francesco Saverio
Membro del Collaboration Group
;
Strano Rossi, Sabina
Supervision
2018

Abstract

Several molecularly imprinted polymers (MIPs) have been synthesized for the first time using various synthetic cannabinoids (JWH007, JWH015 and JWH098) as template molecules. Ethylene dimethacrylate (EDMA) was used as a functional monomer for all cases. Similarly, divinylbenzene (DVB) and 2,2′-azobisisobutyronitrile (AIBN) were used as cross-linker and initiator, respectively. The prepared MIPs have been fully characterized and evaluated as new selective adsorbents for micro-solid phase extraction (μ-SPE) of synthetic cannabinoids in urine. The developed MIP-μ-SPE devices consisted of a polypropylene (PP) porous membrane containing the adsorbent (novel porous membrane protected micro-solid phase extraction based on a cone-shaped device) for operating in batch mode, which allowed a fast and integrated extraction-cleanup procedure. High performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) was used for quantifying the analytes after MIP-μ-SPE. The best performances were obtained for MIPs prepared from JWH015 as a template. Optimum loading conditions were found to be urine pH of 5.0 and adsorption time of 8.0 min under mechanical (orbital-horizontal) stirring at 100 rpm. The composition of the eluting solution consisted of 75:20:5 heptane/2-propanol/ammonium hydroxide. The elution was assisted by ultrasounds (37 kHz, 325 W) for 8.0 min. In addition, studies regarding selectivity have also been addressed for several drugs of abuse under optimized loading/adsorption conditions. Validation of the method showed good precision and analytical recovery by intra-day and inter-day assays (RSD values lower than 7 and 10% for intra-day and inter-day precision, and within the 83–100% range for intra-day and inter-day analytical recovery).
2018
Inglese
Sánchez-González, J., Odoardi, S., Bermejo, A. M., Bermejo-Barrera, P., Romolo, F. S., Moreda-Piñeiro, A., Strano Rossi, S., Development of a micro-solid-phase extraction molecularly imprinted polymer technique for synthetic cannabinoids assessment in urine followed by liquid chromatography–tandem mass spectrometry, <<JOURNAL OF CHROMATOGRAPHY A>>, 2018; 1550 (n/a): 8-20. [doi:10.1016/j.chroma.2018.03.049] [http://hdl.handle.net/10807/119455]
File in questo prodotto:
File Dimensione Formato  
119455.pdf

non disponibili

Tipologia file ?: Versione Editoriale (PDF)
Licenza: Non specificato
Dimensione 2.61 MB
Formato Unknown
2.61 MB Unknown   Visualizza/Apri
STRANO ROSSI.pdf

accesso aperto

Tipologia file ?: Preprint (versione pre-referaggio)
Licenza: Creative commons
Dimensione 1.34 MB
Formato Adobe PDF
1.34 MB Adobe PDF Visualizza/Apri

I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.

Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/10807/119455
Citazioni
  • ???jsp.display-item.citation.pmc??? 2
  • Scopus 44
  • ???jsp.display-item.citation.isi??? 41
social impact