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采用基于微型多环分流器的非低温人工捕集(M-SNAT)调制装置的全二维气相色谱法分析大麻样品。

Comprehensive two-dimensional gas chromatography using a miniaturized multiloop splitter-based non-cryogenic artificial trapping (M-SNAT) modulation device for analysis of cannabis samples.

机构信息

Department of Chemistry, Faculty of Science, Chulalongkorn University, Bangkok 10330, Thailand.

Research Cluster for Cannabis and its Natural Substances, Chulalongkorn University, Bangkok 10330, Thailand; Department of Pharmacognosy and Pharmaceutical Botany, Faculty of Pharmaceutical Sciences, Chulalongkorn University, Bangkok 10330, Thailand.

出版信息

J Pharm Biomed Anal. 2024 Oct 15;249:116395. doi: 10.1016/j.jpba.2024.116395. Epub 2024 Aug 3.

Abstract

Multiloop splitter-based non-cryogenic artificial trapping (M-SNAT) modulation technique was developed, miniaturized and applied in comprehensive two-dimensional gas chromatography (GC×GC) for analysis of cannabis samples. The approach employed deactivated fuse silica (DFS) columns configured into multiple loop splitter system halving the perimeters of the progressively upstream loops. This splitter device was located between the first (D) semi-nonpolar column outlet and a microfluidic Deans switch (DS). Each splitter loop splits a peak into two subpeaks having the same area with different void times. Three loops were then applied resulting in the number of the split subpeaks (n) of 8 for each peak, and retention time differences between any two adjacent subpeaks (∆t) were the same. By applying periodic heartcut event (H/C) within every artificial modulation period (P) of n×∆t, comprehensive split-and-trapped modulation profiles of analytes could be selectively transferred onto the second (D) polar column (30 m) without cryogen consumption. This artificial modulation system was applied for analysis of cannabis samples with enhanced D peak capacity (n∼15). The established method was applied to analyse cannabis extracts using vegetable oils with or without frying process. This reveals 454 different peaks with 76, 92, 35 and 70 specific components specifically observed by using olive oil extraction (OE), fried OE, coconut oil extraction (CE) and fried CE, respectively.

摘要

多环路分流器非低温人工捕集(M-SNAT)调制技术被开发、小型化并应用于全二维气相色谱(GC×GC)分析大麻样品。该方法采用钝化熔硅(DFS)柱,配置成多个环路分流器系统,使逐渐上游环路的周长减半。该分流器装置位于第一根(D)半非极性柱出口和微流道切换阀(DS)之间。每个分流器环路将一个峰分成两个具有相同面积但不同空时的子峰。然后应用三个环路,每个峰的分裂子峰(n)数量为 8,且任意两个相邻子峰之间的保留时间差异(∆t)相同。通过在每个人工调制周期(P)的 n×∆t 内应用周期性的中心切割事件(H/C),可以将分析物的综合分裂和捕集调制谱选择性地转移到第二根(D)极性柱(30m)上,而无需消耗低温冷却剂。该人工调制系统用于分析大麻样品,具有增强的 D 峰容量(n∼15)。该方法用于分析未经油炸和经过油炸过程的蔬菜油中的大麻提取物。结果显示,使用橄榄油提取(OE)、油炸 OE、椰子油提取(CE)和油炸 CE 分别观察到 454 个不同的峰,其中 76、92、35 和 70 个特定成分。

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