The characterisation of the semi-volatile fractions of plant raw materials and derivatives is, in some cases, fundamental in defining their origin, trade value and potential applications. This is true for Frankincense resins whose semi-volatile fraction compositions discriminate samples of different origins and market prices [1]. Similarly, the semi-volatile content of Cannabis sativa L. plant materials determines whether the plant is intended for fibre/seed production, therapeutic purposes or recreational use [2]. Head space solid-phase microextraction (HS-SPME) is extensively used in combination with gas chromatography-mass spectrometry (GC-MS) to analyze volatiles and semivolatiles. However, its relatively low sensitivity with less volatile compounds often requires long sampling times and high temperatures for their extraction. HS-SPME carried out under reduced pressure, also known as vacuum-assisted HS-SPME (Vac-HS-SPME), has been shown to accelerate the extraction rate of those compounds with low volatility (i.e. semi-volatiles) providing higher extraction efficiency and improved sensitivities in shorter sampling times and at reduced temperatures compared to regular HS-SPME [3]. As for regular HS-SPME, Vac-HS-SPME can be online-combined to gas chromatography-mass spectrometry (GC-MS) instrumentation and the only additional step required is air-evacuation of the vial before or after sample introduction [3]. This work explores the application of Vac-HS-SPME combined with GC-MS to characterize the volatile and semi-volatile pattern of solid matrices of plant origin including Frankincense resins and Cannabis sativa samples. The results prove that Vac-HS-SPME can succesfully be applied to complex plant derived solid matrices and show that with a suitable optimisation of the sampling parameters (i.e. sample temperature during the air-evacuation step and sample amount) sampling under vacuum condition enhances the extraction efficiency of semi-volatiles in shorter sampling times without significant losses of the most volatile components during the air-evacuation step. References [1] Niebler J, Buettner A. Chem Biodivers 13, 613 (2016) [2] Citti C, Braghiroli D, Vandelli MA, Cannazza G. J Pharm Biomed Anal 147, 565 (2018) [3] Psillakis E. Anal Chim Acta 986, 12 (2017)

APPLICATION OF VACUUM-ASSISTED HEADSPACE SOLID PHASE MICROEXTRACTION TO CHARACTERISE THE VOLATILE AND SEMI-VOLATILE FRACTIONS OF COMPLEX SOLID PLANT MATRICES

Francesca Capetti;Giulia Mastellone;Patrizia Rubiolo;Carlo Bicchi;Arianna Marengo;Barbara Sgorbini;Cecilia Cagliero
2021

Abstract

The characterisation of the semi-volatile fractions of plant raw materials and derivatives is, in some cases, fundamental in defining their origin, trade value and potential applications. This is true for Frankincense resins whose semi-volatile fraction compositions discriminate samples of different origins and market prices [1]. Similarly, the semi-volatile content of Cannabis sativa L. plant materials determines whether the plant is intended for fibre/seed production, therapeutic purposes or recreational use [2]. Head space solid-phase microextraction (HS-SPME) is extensively used in combination with gas chromatography-mass spectrometry (GC-MS) to analyze volatiles and semivolatiles. However, its relatively low sensitivity with less volatile compounds often requires long sampling times and high temperatures for their extraction. HS-SPME carried out under reduced pressure, also known as vacuum-assisted HS-SPME (Vac-HS-SPME), has been shown to accelerate the extraction rate of those compounds with low volatility (i.e. semi-volatiles) providing higher extraction efficiency and improved sensitivities in shorter sampling times and at reduced temperatures compared to regular HS-SPME [3]. As for regular HS-SPME, Vac-HS-SPME can be online-combined to gas chromatography-mass spectrometry (GC-MS) instrumentation and the only additional step required is air-evacuation of the vial before or after sample introduction [3]. This work explores the application of Vac-HS-SPME combined with GC-MS to characterize the volatile and semi-volatile pattern of solid matrices of plant origin including Frankincense resins and Cannabis sativa samples. The results prove that Vac-HS-SPME can succesfully be applied to complex plant derived solid matrices and show that with a suitable optimisation of the sampling parameters (i.e. sample temperature during the air-evacuation step and sample amount) sampling under vacuum condition enhances the extraction efficiency of semi-volatiles in shorter sampling times without significant losses of the most volatile components during the air-evacuation step. References [1] Niebler J, Buettner A. Chem Biodivers 13, 613 (2016) [2] Citti C, Braghiroli D, Vandelli MA, Cannazza G. J Pharm Biomed Anal 147, 565 (2018) [3] Psillakis E. Anal Chim Acta 986, 12 (2017)
23rd International Symposium on Advances in Extraction Technologies
Alicante - online
30th June-2nd July 2021
Book of abstracts - 23rd International Symposium on Advances in Extraction Technologies
Miguel Ángel Aguirre, Manuel Miró and Lorena Vidal
122
122
Francesca Capetti, Giulia Mastellone, Patrizia Rubiolo, Carlo Bicchi, Arianna Marengo, Barbara Sgorbini, Elefteria Psillakis, Cecilia Cagliero
File in questo prodotto:
Non ci sono file associati a questo prodotto.

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: http://hdl.handle.net/2318/1799304
Citazioni
  • ???jsp.display-item.citation.pmc??? ND
  • Scopus ND
  • ???jsp.display-item.citation.isi??? ND
social impact