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
2021-01-01
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)
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