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利用 LC-串联质谱法测定大麻油基化妆品中的大麻素。

Determination of cannabinoids in hemp oil based cosmetic products by LC-tandem MS.

机构信息

Food and Drug Administration, Ministry of Health and Welfare, Executive Yuan, 161-2 Kunyang St., Nangang Dist., Taipei 11561, Taiwan.

Department of Food Science, National Taiwan Ocean University, Keelung, Taiwan.

出版信息

J Food Drug Anal. 2021 Sep 15;29(3):502-509. doi: 10.38212/2224-6614.3370.

Abstract

Cosmetic products containing hemp seed oil as permitted raw materials required the specific compound delta-9-tetrahydrocannabinol (THC) below 10 μg/g. THC was the main psychoactive constituent of cannabis. Since hemp seed oil became an increasingly popular ingredient in cosmetics over the last few years, an efficient and reliable analytical method for THC and other cannabinoids in cannabis-infused cosmetic products was in need. A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of delta-9-tetrahydrocannabinol (THC), cannabidiol (CBD), and cannabinol (CBN) in hemp seed oil based cosmetic products was developed. Method validation was performed by fertilizing blank samples with analytes and internal standards (THC-d, CBD-d, and CBN-d). Chromatographic method utilized a Xbridge BEH Shield RP18 column with gradient elution containing 10 mM ammonium formate in water and methanol provided successful separation of THC, CBD, and CBN in cosmetic matrix. The combination of MS detection in positive electrospray ionization (ESI) and multiple reaction monitoring (MRM) mode offered rapid run time 13 minutes with limit of quantification (LOQ) of 0.05 μg/g. The intra- and inter-day recoveries were 79.23-114.04% and 83.55-111.61% with spiking levels ranged between 0.05 μg/g and 0.5 μg/g, respectively. Surveillance results of 90 cosmetic products showed 22, 34, and 5 products containing THC (0.06-1777 μg/g), CBD (0.47-37217 μg/g), and CBN (2.2-25.2 μg/g), respectively. This validated method offered accurate, reliable, and fast way for the determination of drug contaminations including THC, CBD, and CBN in cosmetics. The surveillance results for commercial cosmetic products purchased in Taiwan between 2018-2020 provided valuable background references for THC, CBD, and CBN in hemp seed oil based cosmetic products, and could be used for administration purpose.

摘要

含大麻籽油作为允许的原料的化妆品需将特定化合物 δ-9-四氢大麻酚(THC)含量控制在 10μg/g 以下。THC 是大麻的主要精神活性成分。由于大麻籽油在过去几年中成为化妆品中越来越受欢迎的成分,因此需要一种高效可靠的分析方法来检测大麻中添加的化妆品中的 THC 和其他大麻素。建立了一种用于测定大麻籽油基化妆品中 δ-9-四氢大麻酚(THC)、大麻二酚(CBD)和大麻酚(CBN)的液相色谱-串联质谱(LC-MS/MS)方法。通过用分析物和内标物(THC-d、CBD-d 和 CBN-d)对空白样品进行施肥来进行方法验证。色谱方法采用 Xbridge BEH Shield RP18 柱,梯度洗脱,水中含有 10 mM 甲酸铵和甲醇,成功分离了化妆品基质中的 THC、CBD 和 CBN。正电喷雾电离(ESI)和多反应监测(MRM)模式下的 MS 检测相结合,实现了 13 分钟的快速运行时间,定量限(LOQ)为 0.05μg/g。在 0.05μg/g 至 0.5μg/g 的加标水平下,日内和日间回收率分别为 79.23-114.04%和 83.55-111.61%。对 90 种化妆品的监测结果显示,22 种、34 种和 5 种产品分别含有 THC(0.06-1777μg/g)、CBD(0.47-37217μg/g)和 CBN(2.2-25.2μg/g)。该验证方法为测定化妆品中包括 THC、CBD 和 CBN 在内的药物污染提供了准确、可靠和快速的方法。2018-2020 年在台湾购买的商业化妆品监测结果为大麻籽油基化妆品中 THC、CBD 和 CBN 提供了有价值的背景参考,并可用于管理目的。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/62b2/9261791/c52a67cb7447/jfda-29-03-502f1.jpg

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