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<p>This study presents the development of a HiSorb microextraction method coupled with thermal desorption-gas chromatography-mass spectrometry (TD-GC–MS) for analyzing cannabidiol (CBD) in commercial hemp oils. Two HiSorb sorptive coatings were evaluated, triple-phase polydimethylsiloxane (PDMS)/carbon wide-range (CWR)/divinylbenzene (DVB) and double-phase PDMS/CWR, for their extraction efficiencies. The triple-phase HiSorb, combined with water-bath incubation for 2&#xa0;h at 80&#xa0;°C, delivered the highest CBD recovery. The developed HiSorb-TD-GC–MS method showed excellent linearity (<i>R</i><sup>2</sup> = 0.9951), with a method limit of detection (LOD) of 30&#xa0;µg/mL and a limit of quantification (LOQ) of 100&#xa0;µg/mL. The total chromatographic runtime was 11.2&#xa0;min. Precision was satisfactory, with intra-day RSD % ranging from 6.8 to 7.3% and inter-day RSD % ranging from 6.5 to 7.7%. Recoveries at three concentration levels for diluted sample (low 100&#xa0;μg/mL, medium 300&#xa0;μg/mL, high 500&#xa0;μg/mL) ranged from 77.2 to 86.4%. No detectable formation of Δ<sup>9</sup>-THC was observed, confirming that the method does not induce isomerization of CBD during GC analysis. Greenness assessment yielded AGREE = 0.75 (analytical method) and AGREEprep = 0.54 (sample preparation). The developed method was applied to commercial hemp oil samples and revealed no significant statistical difference (<i>p</i> &gt; 0.05) between the label claim and measured CBD concentration in all tested samples. The application of green analytical methods contributes to sustainability by minimizing environmental impact and enhancing resource efficiency.</p> Graphical Abstract <p></p>

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HiSorb-TD-GC–MS analysis of commercial CBD oils

  • 期刊论文

  • 发表日期：

    2026年1月19日

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  • Marios C. Christodoulou,
  • Efstathios A. Elia,
  • Agapios Agapiou

摘要

This study presents the development of a HiSorb microextraction method coupled with thermal desorption-gas chromatography-mass spectrometry (TD-GC–MS) for analyzing cannabidiol (CBD) in commercial hemp oils. Two HiSorb sorptive coatings were evaluated, triple-phase polydimethylsiloxane (PDMS)/carbon wide-range (CWR)/divinylbenzene (DVB) and double-phase PDMS/CWR, for their extraction efficiencies. The triple-phase HiSorb, combined with water-bath incubation for 2 h at 80 °C, delivered the highest CBD recovery. The developed HiSorb-TD-GC–MS method showed excellent linearity (R2 = 0.9951), with a method limit of detection (LOD) of 30 µg/mL and a limit of quantification (LOQ) of 100 µg/mL. The total chromatographic runtime was 11.2 min. Precision was satisfactory, with intra-day RSD % ranging from 6.8 to 7.3% and inter-day RSD % ranging from 6.5 to 7.7%. Recoveries at three concentration levels for diluted sample (low 100 μg/mL, medium 300 μg/mL, high 500 μg/mL) ranged from 77.2 to 86.4%. No detectable formation of Δ9-THC was observed, confirming that the method does not induce isomerization of CBD during GC analysis. Greenness assessment yielded AGREE = 0.75 (analytical method) and AGREEprep = 0.54 (sample preparation). The developed method was applied to commercial hemp oil samples and revealed no significant statistical difference (p > 0.05) between the label claim and measured CBD concentration in all tested samples. The application of green analytical methods contributes to sustainability by minimizing environmental impact and enhancing resource efficiency.

Graphical Abstract