Vacuum-assisted headspace solid-phase microextraction and gas chromatography coupled to mass spectrometry applied to source rock analysis

Pollo, Breno Jorge; Romero-Orejón, Katherine L.; Marsaioli, Anita Jocelyne; Rosa, Paulo de Tarso Vieira e; Augusto, Fábio

doi:10.1016/j.sampre.2021.100001

Cited by 7 publications

(1 citation statement)

References 23 publications

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“…Most recently, researchers have begun to explore Vac‐HS‐SPME sampling for solid samples. These have included extraction of PAHs from sand [8], BTEX from polluted soil [13], terpenoids from frankincense resins [14], butanoic acids in hard cheeses [15], volatiles from raw fish at sub‐ambient temperatures [16], greener sampling methods for oil‐bearing source‐rock analysis [17], one combined technique for analyzing terpenoids and cannabinoids in hemp [18], and flavor and fragrance components in psilocybin and non‐psilocybin mushrooms [19].…”

Section: Introductionmentioning

confidence: 99%

Investigation of operational fundamentals for vacuum‐assisted headspace high‐capacity solid‐phase microextraction and gas chromatographic analysis of semivolatile compounds from a model solid sample

Thomas,

Myers,

Herrington

et al. 2024

J of Separation Science

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Vacuum‐assisted headspace solid‐phase microextraction (Vac‐HS‐SPME) is a technique used to enhance SPME sampling of semi‐volatile organic compounds. Here, it was combined with a high‐capacity SPME Arrow, which features a larger volume of extraction phase and a more rugged configuration than traditional extraction fibers. An in‐depth assessment of the critical parameters was conducted to achieve optimal extraction of representative compounds from a model solid sample matrix (Ottawa sand). Operational fundamentals investigated included the types of seals needed to create a leak‐free environment under vacuum conditions; the magnitude of the vacuum applied and time needed to activate the Vac kinetics; order of sample vial preparation methods (VPMs); and other standard variables associated with extract analysis by gas chromatography‐mass spectrometry. When exploring the limits of sample VPMs, results indicated an ideal workflow requires the solid sample to be spiked before sealing the vial, allow the sample to rest overnight, then apply vacuum at a pressure of ‐677 mbar (out of ‐789 mbar maximum possible vacuum with pump and compressor used), exerted on the vial for 90 s. This work provides the necessary workflow for the optimization of Vac‐HS‐SPME sampling of analytes from solid matrices.

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