Myers Colton, Herrington Jason S, Hamrah Paul, Anderson Kelsey
Restek Corporation, Bellefonte, PA, United States.
Verity Analytics, San Diego, CA, United States.
Front Chem. 2021 Apr 1;9:619770. doi: 10.3389/fchem.2021.619770. eCollection 2021.
The cannabis market is expanding exponentially in the United States. As state-wide legalization increases, so do demands for analytical testing methodologies. One of the main tests conducted on cannabis products is the analysis for terpenes. This research focused on implementation of accelerated solvent extraction (ASE), utilizing surrogate matrix matching, and evaluation of traditional vs. more modern sample introduction techniques for analyzing terpenes via gas chromatography-mass spectrometry (GC-MS). Introduction techniques included Headspace-Syringe (HS-Syringe), HS-Solid Phase Microextraction Arrow (HS-SPME Arrow), Direct Immersion-SPME Arrow (DI-SPME Arrow), and Liquid Injection-Syringe (LI-Syringe). The LI-Syringe approach was deemed the most straightforward and robust method with terpene working ranges of 0.04-5.12 μg/mL; values of 0.988-0.996 (0.993 average); limit of quantitation values of 0.017-0.129 μg/mL (0.047 average); analytical precisions of 2.58-9.64% RSD (1.56 average); overall ASE-LI-Syringe-GC-MS method precisions of 1.73-14.6% RSD (4.97 average); and % recoveries of 84.6-98.9% (90.2 average) for the 23 terpenes of interest. Sample workflows and results are discussed, with an evaluation of the advantages/limitations of each approach and opportunities for future work.
大麻市场在美国正呈指数级扩张。随着全州范围内大麻合法化程度的提高，对分析检测方法的需求也在增加。对大麻产品进行的主要检测之一是萜烯分析。本研究聚焦于加速溶剂萃取（ASE）的实施，采用替代基质匹配，并评估传统与更现代的样品引入技术，以通过气相色谱 - 质谱联用（GC - MS）分析萜烯。引入技术包括顶空进样 - 注射器（HS - 注射器）、顶空固相微萃取箭头（HS - SPME箭头）、直接浸入式SPME箭头（DI - SPME箭头）和液体进样 - 注射器（LI - 注射器）。LI - 注射器方法被认为是最直接且稳健的方法，其萜烯工作范围为0.04 - 5.12μg/mL；相关系数值为0.988 - 0.996（平均0.993）；定量限为0.017 - 0.129μg/mL（平均0.047）；分析精密度为2.58 - 9.64%RSD（平均1.56）；整体ASE - LI - 注射器 - GC - MS方法精密度为1.73 - 14.6%RSD（平均4.97）；对于23种目标萜烯的回收率为84.6 - 98.9%（平均90.2）。文中讨论了样品工作流程和结果，并评估了每种方法的优缺点以及未来工作的机会。
