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硅胶 TLC 与银(I)保留区和显色智能手机检测对半定量筛查大麻素类似物。

Semiquantitative Screening of THC Analogues by Silica Gel TLC with an Ag(I) Retention Zone and Chromogenic Smartphone Detection.

机构信息

Key Laboratory of Phytochemical R&D of Hunan Province and Key Laboratory of Chemical Biology & Traditional Chinese Medicine Research of Ministry of Education, Hunan Normal University, Changsha410081, China.

Laboratory of Organic Chemistry, Wageningen University, Wageningen6708 WE, The Netherlands.

出版信息

Anal Chem. 2022 Oct 11;94(40):13710-13718. doi: 10.1021/acs.analchem.2c01627. Epub 2022 Sep 30.

Abstract

With the ever-evolving cannabis industry, low-cost and high-throughput analytical methods for cannabinoids are urgently needed. Normally, (potentially) psychoactive cannabinoids, typically represented by Δ9-tetrahydrocannabinol (Δ9-THC), and nonpsychoactive cannabinoids with therapeutic benefits, typically represented by cannabidiol (CBD), are the target analytes. Structurally, the former (tetrahydrocannabinolic acid (THCA), cannabinol (CBN), and THC) have one olefinic double bond and the latter (cannabidiolic acid (CBDA), cannabigerol (CBG), and CBD) have two, which results in different affinities toward Ag(I) ions. Thus, a silica gel thin-layer chromatography (TLC) plate with the lower third impregnated with Ag(I) ions enabled within minutes a digital chromatographic separation of strongly retained CBD analogues and poorly retained THC analogues. The resolution () between the closest two spots from the two groups was 4.7, which is almost 8 times higher than the resolution on unmodified TLC. After applying Fast Blue BB as a chromogenic reagent, smartphone-based color analysis enabled semiquantification of the total percentage of THC analogues (with a limit of detection (LOD) of 11 ng for THC, 54 ng for CBN, and 50 ng for THCA when the loaded volume is 1.0 μL). The method was validated by analyzing mixed cannabis extracts and cannabis extracts. The results correlated with those of high-performance liquid chromatography with ultraviolet detection (HPLC-UV) ( = 0.97), but the TLC approach had the advantages of multi-minute analysis time, high throughput, low solvent consumption, portability, and ease of interpretation. In a desiccator, Ag(I)-TLC plates can be stored for at least 3 months. Therefore, this method would allow rapid distinction between high and low THC varieties of cannabis, with the potential for on-site applicability.

摘要

随着大麻产业的不断发展,人们迫切需要低成本、高通量的大麻分析方法。通常情况下,(潜在)具有精神活性的大麻素,通常以 Δ9-四氢大麻酚(Δ9-THC)为代表,以及具有治疗益处的非精神活性大麻素,通常以大麻二酚(CBD)为代表,是目标分析物。从结构上看,前者(四氢大麻酸(THCA)、大麻酚(CBN)和 THC)有一个烯烃双键,而后者(大麻二酚酸(CBDA)、大麻萜酚(CBG)和 CBD)有两个,这导致它们对 Ag(I)离子的亲和力不同。因此,几分钟内就可以通过硅胶薄层色谱(TLC)板的下三分之一部分负载 Ag(I)离子,实现对强保留 CBD 类似物和弱保留 THC 类似物的数字色谱分离。两组中最近两个斑点之间的分辨率()为 4.7,几乎是未修饰 TLC 的分辨率的 8 倍。使用 Fast Blue BB 作为显色试剂后,基于智能手机的颜色分析能够对半定量分析 THC 类似物的总百分比(当加载体积为 1.0 μL 时,THC 的检测限(LOD)为 11 ng,CBN 的 LOD 为 54 ng,THCA 的 LOD 为 50 ng)。该方法通过分析混合大麻提取物和大麻提取物进行了验证。结果与高效液相色谱-紫外检测(HPLC-UV)的结果相关( = 0.97),但 TLC 方法具有分析时间长、高通量、低溶剂消耗、便携性和易于解释的优点。在干燥器中,Ag(I)-TLC 板至少可以保存 3 个月。因此,该方法可以快速区分 THC 含量高和低的大麻品种,具有现场适用性的潜力。

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