Key Laboratory of Phytochemical R&D of Hunan Province and Key Laboratory of Chemical Biology & Traditional Chinese Medicine Research of Ministry of Education, Hunan Normal University, Changsha 410081, China.
Laboratory of Organic Chemistry, Wageningen University, Wageningen 6708 WE, The Netherlands.
Anal Chem. 2021 Mar 2;93(8):3794-3802. doi: 10.1021/acs.analchem.0c04270. Epub 2021 Feb 12.
The control over the amount of psychoactive THC (Δ-9-tetrahydrocannabinol) in commercial cannabidiol (CBD) products has to be strict. A fast and simple semiquantitative Ag(I)-impregnated paper spray mass spectrometric method for differentiating between THC and CBD, which show no difference in standard single-stage or tandem MS, was established. Because of a different binding affinity to Ag(I) ions, quasi-molecular Ag(I) adducts [THC + Ag] and [CBD + Ag] at / 421 and 423 give different fragmentation patterns. The product ions at / 313 for THC and / 353 and 355 for CBD can be used to distinguish THC and CBD and to determine their ratio. Quantification of THC/CBD ratios in commercial CBD oils was accomplished with a low matrix effect (-2.2 ± 0.4% for THC and -2.0 ± 0.3% for CBD). After simple methanol extraction (recovery of 87.3 ± 1.2% for THC and 92.3 ± 1.4% for CBD), Ag(I)-impregnated paper spray analysis was employed to determine this ratio. A single run can be completed in a few minutes. This method was benchmarked against the UHPLC-UV method. Ag(I)-impregnated paper spray MS had the same working range (THC/CBD = 0.001-1) as UHPLC-UV analysis ( = 0.9896 and = 0.9998, respectively), as well as comparable accuracy (-2.7 to 14%) and precision (RSD 1.7-11%). The method was further validated by the analysis of 10 commercial oils by Ag(I)-impregnated paper spray MS and UHPLC-UV analysis. Based on the determined relative concentration ratios of THC/CBD and the declared CBD concentration, 6 out of 10 CBD oils appear to contain more THC than the Dutch legal limit of 0.05%.
商业大麻二酚 (CBD) 产品中精神活性成分四氢大麻酚 (Δ-9-四氢大麻酚) 的含量必须严格控制。本研究建立了一种快速简单的半定量 Ag(I)浸渍纸喷雾质谱法，用于区分 THC 和 CBD，标准单级或串联 MS 无差异。由于与 Ag(I)离子的结合亲和力不同，准分子 Ag(I)加合物 [THC + Ag] 和 [CBD + Ag] 在 / 421 和 423 处给出不同的碎裂模式。THC 的产物离子为 / 313，CBD 的产物离子为 / 353 和 355，可用于区分 THC 和 CBD，并确定它们的比例。采用低基质效应（THC 为-2.2 ± 0.4%，CBD 为-2.0 ± 0.3%）对商业 CBD 油中的 THC/CBD 比值进行定量。经过简单的甲醇提取（THC 的回收率为 87.3 ± 1.2%，CBD 的回收率为 92.3 ± 1.4%），采用 Ag(I)浸渍纸喷雾分析来测定该比值。几分钟内即可完成单次运行。该方法与 UHPLC-UV 方法进行了基准测试。Ag(I)浸渍纸喷雾 MS 与 UHPLC-UV 分析具有相同的工作范围（THC/CBD = 0.001-1）（分别为 = 0.9896 和 = 0.9998），以及相当的准确性（-2.7 至 14%）和精密度（RSD 为 1.7-11%）。进一步通过 10 种商业油的 Ag(I)浸渍纸喷雾 MS 和 UHPLC-UV 分析验证了该方法。基于测定的 THC/CBD 相对浓度比和宣称的 CBD 浓度，10 种 CBD 油中有 6 种似乎含有超过荷兰法定限量 0.05%的 THC。
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