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乳化化妆品中大麻二酚测定的挑战以及固相萃取结合高效液相色谱-紫外-串联质谱联用的应用

Challenges of cannabidiol determination in emulsified cosmetics and application of solid-phase extraction followed by HPLC-UV-MS/MS.

作者信息

Vágnerová Magdaléna, Sýkora David, Nemeškalová Alžběta, Kuchař Martin

机构信息

Department of Analytical Chemistry, University of Chemistry and Technology, Technická 5, 166 28, Prague 6, Prague, Czech Republic.

Forensic Laboratory of Biologically Active Substances, Department of Chemistry of Natural Compounds, University of Chemistry and Technology, Technická 5, 166 28, Prague 6, Prague, Czech Republic.

出版信息

Anal Bioanal Chem. 2025 Mar;417(6):1153-1163. doi: 10.1007/s00216-024-05716-9. Epub 2025 Jan 7.

DOI:10.1007/s00216-024-05716-9
PMID:39762637
Abstract

The recent surge in popularity of cannabidiol-infused products extends beyond food and supplements to the cosmetic industry. Accurate labeling remains a significant concern, as many products fail to meet advertised cannabidiol content and/or contain psychoactive tetrahydrocannabinol above the permissible levels. In this work, we present the use of an HPLC-UV-MS/MS method for the quantification of five major cannabinoids (cannabidiol, cannabidiolic acid, tetrahydrocannabinol, tetrahydrocannabinolic acid, and cannabigerol) in oil-in-water cosmetic emulsions. The sample extraction is based on dispersing the sample in isopropanol, followed by solid-phase extraction using Bond Elut Plexa PAX cartridge. The viability of this method is demonstrated by comparing matrix effects in samples subjected to solid-phase extraction (0‒11% suppression of cannabidiol ionization) to samples extracted without additional purification steps (0‒84% ionization suppression of cannabidiol ionization). The limit of quantification is determined at 0.1 mg/g and the calibration is employed in the range of 0.1‒50 mg/g for cannabidiol and 0.1‒10 mg/g for all other analytes. Finally, 36 real cosmetic samples from the Czech market were analyzed. Of these, 14 indicated the amount of CBD on the label but only five (36%) were accurate, i.e., within 90‒110% of the labeled amount, and a considerable amount of THC (0.16 ± 0.01 mg/g) was found in one sample. These findings contribute to the cumulating evidence that cannabidiol-based consumer products are often mislabeled and highlight the importance of better regulatory compliance.

摘要

最近,含大麻二酚产品的人气飙升,其应用范围已从食品和补充剂扩展到化妆品行业。准确标注仍是一个重大问题,因为许多产品未达到所宣称的大麻二酚含量,和/或含有超过许可水平的具有精神活性的四氢大麻酚。在这项工作中,我们展示了一种高效液相色谱 - 紫外 - 串联质谱法,用于定量水包油型化妆品乳液中的五种主要大麻素(大麻二酚、大麻二酚酸、四氢大麻酚、四氢大麻酚酸和大麻萜酚)。样品提取是基于将样品分散在异丙醇中,然后使用Bond Elut Plexa PAX柱进行固相萃取。通过比较经过固相萃取的样品(大麻二酚离子化抑制0‒11%)与未经额外纯化步骤提取的样品(大麻二酚离子化抑制0‒84%)中的基质效应,证明了该方法的可行性。大麻二酚的定量限为0.1 mg/g,校准范围为0.1‒50 mg/g,其他所有分析物的校准范围为0.1‒10 mg/g。最后,对来自捷克市场的36个真实化妆品样品进行了分析。其中,14个样品在标签上标明了大麻二酚含量,但只有5个(36%)是准确的,即含量在标签标注量的90‒110%范围内,并且在一个样品中发现了相当数量的四氢大麻酚(0.16 ± 0.01 mg/g)。这些发现进一步证明了以大麻二酚为基础的消费品经常被误标,并凸显了更好地遵守监管规定的重要性。

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JAMA Netw Open. 2022 Jul 1;5(7):e2223019. doi: 10.1001/jamanetworkopen.2022.23019.
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J Food Drug Anal. 2021 Sep 15;29(3):502-509. doi: 10.38212/2224-6614.3370.
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Cannabidiol (CBD) product contamination: Quantitative analysis of Δ-tetrahydrocannabinol (Δ-THC) concentrations found in commercially available CBD products.
大麻二酚 (CBD) 产品污染:市售 CBD 产品中发现的 Δ-四氢大麻酚 (Δ-THC) 浓度的定量分析。
Drug Alcohol Depend. 2022 Aug 1;237:109522. doi: 10.1016/j.drugalcdep.2022.109522. Epub 2022 Jun 3.
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J Cannabis Res. 2022 Jun 6;4(1):28. doi: 10.1186/s42238-022-00140-1.
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