Ciolino Laura A, Ranieri Tracy L, Taylor Allison M
Forensic Chemistry Center, Food and Drug Administration, 6751 Steger Drive, Cincinnati, OH, USA.
Forensic Sci Int. 2018 Aug;289:429-437. doi: 10.1016/j.forsciint.2018.05.032. Epub 2018 Jun 6.
The recent surge in the sale of cannabis-based consumer products in the US includes foods, candies, beverages, topicals, vapes/eliquids, oral supplements in various forms, recreational marijuana plants, and plant extracts or preparations. The wide variety of product and sample types has resulted in a host of new matrix interferences when conducting qualitative testing for the cannabis cannabinoids such as cannabidiol and d9-tetrahydrocannabinol. A qualitative GC-MS method is presented in this work, which uses a commercial 35% silphenylene phase to provide chromatographic resolution for 11 target cannabinoids as their trimethylsilyl derivatives (CBD, CBDA, d9THC, THCA, CBN, d8THC, CBG, CBGA, CBDV, THCV, and CBC). The method uses variants of ethanol- and acetonitrile-based extractants to successfully minimize or eliminate several types of interferents, and also provides protocols to address specific interferents such as glycerin and lactose. Method validation included spike/recovery for five cannabinoids of primary interest (spiking level 50μg/g) from a series of edible oils, foods, beverages, candies, topicals, oral OTC pharmaceuticals, glycerin, and propylene glycol. The minimum detectable concentration was established as 1.0μg/g. The method was applied to about sixty diverse commercial products, as well as to recreational marijuana plants, plant preparations, hempseed oils, and dronabinol capsules.
近期美国基于大麻的消费品销量激增,这些产品包括食品、糖果、饮料、外用制剂、电子烟油/电子烟液、各种形式的口服补充剂、娱乐用大麻植株以及植物提取物或制剂。产品和样品类型繁多,在对大麻素(如大麻二酚和Δ⁹-四氢大麻酚)进行定性检测时,产生了许多新的基质干扰。本文介绍了一种定性气相色谱-质谱联用方法,该方法使用一种市售的35%硅亚苯基固定相,以其三甲硅烷基衍生物形式为11种目标大麻素(CBD、CBDA、Δ⁹THC、THCA、CBN、Δ⁸THC、CBG、CBGA、CBDV、THCV和CBC)提供色谱分离度。该方法使用基于乙醇和乙腈的萃取剂变体,成功地减少或消除了几种干扰物类型,还提供了处理甘油和乳糖等特定干扰物的方案。方法验证包括对一系列食用油、食品、饮料、糖果、外用制剂、口服非处方药品、甘油和丙二醇中五种主要感兴趣的大麻素(加标水平50μg/g)进行加标回收实验。最低检测浓度确定为1.0μg/g。该方法应用于约60种不同的商业产品,以及娱乐用大麻植株、植物制剂、大麻籽油和屈大麻酚胶囊。