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采用 LC 分析富含大麻二酚的产品,结合使用紫外和 MS/MS 检测方法。

Combination of UV and MS/MS detection for the LC analysis of cannabidiol-rich products.

机构信息

Department of Analytical Chemistry, University of Chemistry and Technology Prague, Technická 5, 166 28, Prague 6, Czech Republic; Forensic Laboratory of Biologically Active Substances, Department of Chemistry of Natural Compounds, University of Chemistry and Technology Prague, Technická 5, 166 28, Prague 6, Czech Republic; National Institute of Mental Health, Topolová 748, 250 67, Klecany, Czech Republic.

Forensic Laboratory of Biologically Active Substances, Department of Chemistry of Natural Compounds, University of Chemistry and Technology Prague, Technická 5, 166 28, Prague 6, Czech Republic; National Institute of Mental Health, Topolová 748, 250 67, Klecany, Czech Republic.

出版信息

Talanta. 2020 Nov 1;219:121250. doi: 10.1016/j.talanta.2020.121250. Epub 2020 Jun 17.

DOI:10.1016/j.talanta.2020.121250
PMID:32887141
Abstract

Cannabidiol (CBD), a major non-psychoactive cannabinoid, has received a lot of attention due to its potential anti-inflammatory, pain-relieving, and anti-anxiety properties. This has led to a recent boom in CBD-rich commercial products, which are sold without prescription in the form of oils, candies, and cosmetics. Since these products are derived from cannabis, the presence of the psychoactive tetrahydrocannabinol (THC) has to be tested before they enter the market. Here, we present a high-throughput approach based on liquid chromatography coupled to UV and tandem mass spectrometric detection for the determination of CBD, THC, and six other minor cannabinoids (cannabigerolic acid, cannabidivarin, cannabinol, cannabigerol, cannabidiolic acid, and tetrahydrocannabinolic acid) in a wide range of concentrations and in a variety of matrices, including oils, hydrophobic ointments, water-soluble liquids, plant material and gelatinous gummies. Each product was dissolved in a suitable solvent and further diluted to avoid matrix interference. The diluted samples were analyzed by reversed-phase chromatography, coupled to a UV detector followed by a triple quadrupole mass spectrometer, used in the multiple reaction monitoring mode. The UV signal was utilized for the quantification of samples containing high levels of CBD, while the mass spectrometer was used for low levels of THC and other minor cannabinoids. This allowed us to meet the required sensitivity for THC while significantly expanding the range of analyzed CBD, all within an 8-min long chromatographic run. The samples were further quantified using calibration in solvent, the approach was validated, and the validation criteria were met for all matrices except for two (i.e., emulsions and gels). The lower limit of quantification for THC was 0.5 μg/g in gummies, 1.0 μg/g in oils, ointments and liquids, and 5.0 μg/g in plant material. CBD was analyzed in the range of 0.5-60,000 μg/g in gummies, 1-120,000 μg/g in oils, ointments and liquids, and 5-300,000 μg/g in plant material. The developed method was used for the analysis of thirteen real products with a wide range of CBD content, with positive THC findings in twelve of them.

摘要

大麻二酚(CBD)是一种主要的非精神活性大麻素,由于其具有潜在的抗炎、止痛和抗焦虑特性,因此备受关注。这导致富含 CBD 的商业产品最近出现热潮,这些产品以油、糖果和化妆品的形式无需处方即可销售。由于这些产品源自大麻,因此在进入市场之前必须检测其是否含有精神活性四氢大麻酚(THC)。在这里,我们提出了一种基于液相色谱-紫外和串联质谱检测的高通量方法,用于测定 CBD、THC 和其他六种微量大麻素(大麻萜酚酸、大麻二酚、大麻酚、大麻二酚、大麻酸和四氢大麻酚酸)的广泛浓度和各种基质,包括油、疏水性软膏、水溶性液体、植物材料和胶凝 gummies。每种产品都溶解在合适的溶剂中,并进一步稀释以避免基质干扰。稀释后的样品通过反相色谱分析,与紫外检测器串联,然后与三重四极杆质谱仪在多反应监测模式下联用。紫外信号用于定量 CBD 含量高的样品,而质谱仪用于 THC 和其他微量大麻素的低含量分析。这使得我们能够满足 THC 的灵敏度要求,同时显著扩大了分析 CBD 的范围,所有这些都在 8 分钟的色谱运行内完成。使用溶剂校准对样品进行进一步定量,验证了该方法,并满足了所有基质的验证标准,除了两种基质(即乳液和凝胶)。在 gummies 中,THC 的定量下限为 0.5 μg/g,在油、软膏和液体中为 1.0 μg/g,在植物材料中为 5.0 μg/g。在 gummies 中分析 CBD 的范围为 0.5-60000 μg/g,在油、软膏和液体中为 1-120000 μg/g,在植物材料中为 5-300000 μg/g。该方法用于分析 13 种具有广泛 CBD 含量的真实产品,其中 12 种产品检测到 THC 呈阳性。

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