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建立 UHPLC/DAD 法测定缴获物中大麻素的方法学验证:对在比利时 CBD 商店销售的 213 个样本进行分析。

Validation of an UHPLC/DAD method for the determination of cannabinoids in seized materials: Analysis of 213 samples sold in Belgian CBD shops.

机构信息

Laboratory of Clinical, Forensic and Environmental Toxicology, Center for Interdisciplinary Research on Medicines (CIRM), University of Liege, Belgium.

Laboratory of Clinical, Forensic and Environmental Toxicology, Center for Interdisciplinary Research on Medicines (CIRM), University of Liege, Belgium.

出版信息

Forensic Sci Int. 2020 May;310:110234. doi: 10.1016/j.forsciint.2020.110234. Epub 2020 Mar 3.

Abstract

PURPOSE

Nowadays, (-)-cannabidiol (CBD) is gaining popularity for the treatment of various problems and can be found easily in many stores in Belgium. However, such product must comply with the law: if the total tetrahydrocannabinol (THC) content [(-)-Δ9-tetrahydrocannabinol + (-)-Δ9-tetrahydrocannabinolic acid A (THC-A)] is higher than 0.2%, it is considered as narcotic by the Belgian legislation. In this context, we have developed a method to quantify major cannabinoids (THC, THC-A, CBD, cannabidiolic acid, cannabigerolic acid, cannabigerol and cannabinol) in plant material.

METHODS

After drying, a liquid-liquid extraction was performed on plant materials, followed by dilutions. Extracts were analyzed by ultra-high-performance liquid chromatography combined with a photodiode array detector. Mobile phases consisted of methanol and 0.1% formic acid in water applied in a 16-minute gradient mode. After validating the method, it was applied to 213 samples seized by the police in CBD shops.

RESULTS

The method fulfilled the criteria in terms of specificity, calibration curve, precision, trueness and dosing range. Total THC content ranged from 0.14 to 1.17% (median 0.38%) with 110 samples exceeding the Belgian legal threshold of 0.2%. The amounts measured in the samples varied greatly, some were 6 times below the amount labelled on the packaging, others showed a concentration 4 times higher than stated on the package. Same strain also showed concentration differences from shop to shop.

CONCLUSION

Our method was successfully validated and applied to samples seized in CBD shops. Half of the products exceeded the Belgian legal threshold. THC and CBD concentrations discrepancies showed that products sold in CBD shops are not pharmaceutical grade.

摘要

目的

如今,(-)-大麻二酚(CBD)因其可用于治疗各种疾病而广受欢迎,在比利时的许多商店都很容易买到。但是,此类产品必须符合法律规定:如果总四氢大麻酚(THC)含量[(-)-Δ9-四氢大麻酚+(-)-Δ9-四氢大麻酚酸 A(THC-A)]超过 0.2%,则根据比利时法律,此类产品将被视为麻醉品。在这种情况下,我们开发了一种方法来定量测定植物材料中的主要大麻素(THC、THC-A、CBD、大麻二酚酸、大麻萜酚酸、大麻萜酚和大麻酚)。

方法

对植物材料进行干燥后,进行液-液萃取,然后进行稀释。采用超高效液相色谱法与光电二极管阵列检测器相结合的方法对提取物进行分析。流动相由甲醇和 0.1%甲酸在水中组成,采用 16 分钟梯度模式。方法验证后,对警方从 CBD 商店缴获的 213 个样品进行了分析。

结果

该方法在专属性、校准曲线、精密度、准确度和剂量范围方面均符合标准。总 THC 含量范围为 0.14%至 1.17%(中位数为 0.38%),其中 110 个样品超过了比利时 0.2%的法定阈值。样品中测量的含量差异很大,有些样品的含量比包装上标注的低 6 倍,有些样品的含量比包装上标注的高 4 倍。同一品种在不同商店的浓度也存在差异。

结论

我们的方法成功地进行了验证,并应用于 CBD 商店缴获的样品。一半的产品超过了比利时的法定阈值。THC 和 CBD 浓度的差异表明,在 CBD 商店销售的产品不是医药级的。

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