Cross Category Research and Innovation Department, Global Technology Center, Colgate-Palmolive Company, 909 River Road, Piscataway, New Jersey 08855, United States.
J Am Soc Mass Spectrom. 2021 Aug 4;32(8):1919-1927. doi: 10.1021/jasms.0c00331. Epub 2020 Nov 23.
The cannabis analysis has gained new importance worldwide due to the rapid expansion of the hemp global market. Many reverse phase high performance liquid chromatography (HPLC) methods have been developed to analyze cannabidiol (CBD) and its analogues due to the nice fit with their log P values at around 6. However, when CBD was blended with hemp seed oil in consumer, cosmetic, and food industries, the high content of triacylglycerides (TAGs) from hemp seed oil were retained and accumulated inside C columns with the common mobile phases and caused a column pressure increase and ghost peaks after continuous sample injections. Coupled with the chemical profile from high resolution mass spectrometry (HRMS) detection, a novel hydrophilic interaction liquid chromatography (HILIC) CBD quantitation method was developed, specifically for CBD blended hemp seed oil materials, which can overcome the matrix buildup in reverse phase columns. The zwitterionic (ZIC)-cHILIC column containing a dense water layer on the stationary phase surface provided a stable partitioning separation mechanism to separate the CBD from TAGs in hemp seed oil. This water layer favors the sustaining NHF buffer ions, which can maximize the salting-out action and help reduce the adsorptive interaction between TAGs and stationary phase sulfobetaine materials. The high percentage of acetonitrile (99%) contributed to method sensitivity and reduced instrument maintenance time. The method was developed and validated for the first time. It has been successfully applied to quantify CBD content in hemp seed oil samples, thus demonstrating it to be a useful tool for both quality control and safety assurance in CBD hemp seed oil raw materials and related products.
由于大麻全球市场的迅速扩张，大麻分析在全球范围内变得愈发重要。许多反相高效液相色谱（HPLC）方法已经被开发出来，以分析大麻二酚（CBD）及其类似物，这是因为它们的 log P 值在 6 左右，与 CBD 非常吻合。然而，当 CBD 与麻籽油混合在消费者、化妆品和食品行业中时，麻籽油中的大量三酰基甘油（TAGs）会被保留下来，并在普通流动相和连续进样后在 C 柱内积累，导致柱压升高和鬼峰出现。结合高分辨率质谱（HRMS）检测的化学特征，开发了一种新型亲水作用液相色谱（HILIC）CBD 定量方法，专门用于 CBD 混合麻籽油材料，可以克服反相柱中的基质堆积问题。含有固定相表面致密水层的两性离子（ZIC）-cHILIC 柱提供了一种稳定的分配分离机制，可将 CBD 与麻籽油中的 TAGs 分离。这层水有利于维持 NHF 缓冲离子，最大程度地发挥盐析作用，并有助于减少 TAGs 与固定相磺基甜菜碱材料之间的吸附相互作用。高比例的乙腈（99%）有助于提高方法的灵敏度并减少仪器维护时间。该方法是首次开发和验证的。它已成功应用于定量分析麻籽油样品中的 CBD 含量，因此证明它是 CBD 麻籽油原料和相关产品质量控制和安全保证的有用工具。
