{"_":"评估用于LC分离Δ-THC及其他相关大麻素的不同C色谱柱.","sub":["18"],"sup":["9"]}

摘要(中文译文)

在复杂样品中通过液相色谱法（LC）实现δ-9-四氢大麻酚（Δ-THC）的最佳分离尤为具有挑战性，原因在于其他大麻素类化合物的潜在干扰。在植物样品中已检测到超过100种大麻素类化合物。大麻来源的成品中Δ-THC的分离被认为比植物提取物更易于一次性分析，因为在材料制备过程中酸性大麻素类化合物会转化为其中性形式。然而，合成或半合成大麻素产品的出现，如δ-8-四氢大麻酚（Δ-THC），由于合成副产物的存在导致了更多的色谱干扰。美国国家标准与技术研究院（NIST）化学科学部（CSD）最初采用的液相色谱分离方法在存在这些色谱干扰时无法满足要求。在此背景下，本文所展示的工作探索了使用不同的单体型和聚合型十八烷基硅烷（C）色谱柱通过液相色谱对11种大麻素混合物进行初步分离。这些色谱柱使用标准参考物质869b作为三组分柱选择性测试混合物进行表征，以确定LC C色谱柱被归类为单体型还是聚合型。单体型C色谱柱（NexLeaf C、ACE 3 C和ACE Super C）对11种大麻素提供了更好的分离效果，在对流动相程序进行微调后，可在13分钟内获得基线分离。使用NexLeaf C LC-UV方法，分析了Δ-THC与四种已知色谱干扰物的混合物。大麻酚酸（CBNA）无法与Δ-THC分离；然而，CBNA与Δ-THC的吸收光谱差异显著，使用光电二极管阵列检测可以轻松识别这些大麻素类化合物的共洗脱。当CBNA存在时，可使用本文开发的替代NexLeaf C LC-UV方法对样品进行重新分析，该方法可在60分钟内实现Δ-THC与CBNA的基线分离。这两种LC-UV方法将在NIST CSD通过未来的出版物中的定量比较进一步评估，从而使其能够用于植物和/或大麻来源成品的标准参考物质开发。

Abstract

The best separation possible of delta-9-tetrahydrocannabinol (Δ-THC) in complex samples via liquid chromatography (LC) is particularly challenging due to the potential for interference from other cannabinoids. Over 100 cannabinoids have been detected in plant samples. The separation of Δ-THC in -derived finished products was believed to be easier than plant extracts to analyze at one time because the acidic cannabinoids are converted to their neutral cannabinoids during material preparation. However, the emergence of synthetic or semi-synthetic cannabinoid products, such as delta-8-tetrahydrocannabinol (Δ-THC), has led to more chromatographic interferences due to the presence of synthetic by-products. The original LC separation method implemented in the Chemical Sciences Division (CSD) at the National Institute of Standards and Technology (NIST) was not acceptable when these chromatographic interferences were present. Within this context, the work presented here explores initial separation of an 11 cannabinoid mixture using different monomeric and polymeric octadecylsilane (C) columns via liquid chromatography. These columns were characterized using the Standard Reference Material 869b as a three-component column selectivity test mixture to determine if an LC C column is classified as monomeric or polymeric. Monomeric C columns (NexLeaf C, ACE 3 C, and ACE Super C) provided better separations of the 11 cannabinoids, and baseline separations were obtained in less than 13 min after minor adjustments to the mobile phase program. Using the NexLeaf C LC-UV method, mixtures of Δ-THC and four known chromatographic interferences were analyzed. Cannabinolic acid (CBNA) could not be separated from Δ-THC; however, CBNA has drastically different absorbance spectra from Δ-THC, and the co-elution of these cannabinoids can easily be recognized using photodiode array detection. When CBNA is present, the sample can be reanalyzed using an alternate NexLeaf C LC-UV method developed here, which baseline-resolves Δ-THC and CBNA in 60 min. These two LC-UV methods will be further evaluated at NIST CSD through quantitative comparisons in future publications, enabling their use in the development of reference materials for plants and/or -derived finished products.

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