Direct sample introduction in high-performance liquid chromatography analysis of oily medicinal cannabis samples using surfactant-free microemulsion

Ana Paula Lamounier, Bárbara da Conceição Coelho Cotta Cardoso, Alessandra Licursi Maia Cerqueira da Cunha
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Abstract

The therapeutic use of medicinal Cannabis has raised challenges in quality control and cannabinoid quantification in oil extracts, primarily due to incompatibility with liquid chromatography systems. Surfactant-free microemulsion (SFME) systems offer a promising, efficient, and sustainable solution, enabling direct analysis by high-performance liquid chromatography. These microemulsions are dispersions of two immiscible liquids, typically oil and water, made compatible by an amphiphilic substance that interacts with both polar and nonpolar fractions. After SFME testing and critical analysis of the results, clear and homogeneous microemulsions were observed regardless of the oil-to-water ratio studied, provided that sufficient quantities of 1-octanol:1-propanol (3:10 v/v) were added. Based on the established robust working range, the 1:2 (oil:ultrapure water) ratio (% w/w) was chosen as the compromise condition, minimizing medicinal oil use while ensuring compatibility with the chromatographic system. Univariate optimization of chromatographic conditions enabled simultaneous analysis of five cannabinoids, including cannabidiol (CBD), cannabidiolic acid (CBDA), tetrahydrocannabutol (THCB), cannabinol (CBN), and tetrahydrocannabinol (Δ9-THC) using a ZORBAX Eclipse Plus C18 column at 35 °C. The method employed isocratic elution with a mobile phase of 82:18 %v/v methanol:ultrapure water containing 0.15 ± 0.05 % v/v formic acid, a 1.0 mL min−1 flow rate, and a 20 μL injection volume, using the fluorescence and UV absorption detectors. This proposal offers sensitivity (LOD in the ng mL−1), selectivity, and separation efficiency, associated with low cost, minimal waste generation, and low energy demand, aligning with Green Chemistry principles.
使用无表面活性剂微乳液对含油药用大麻样品进行高效液相色谱分析,直接进样
药用大麻的治疗用途在油提取物的质量控制和大麻素定量方面提出了挑战,主要是由于与液相色谱系统不相容。无表面活性剂微乳液(SFME)系统提供了一种有前途的、高效的、可持续的解决方案,可以通过高效液相色谱进行直接分析。这些微乳液是两种不相容的液体(通常是油和水)的分散体,通过与极性和非极性组分相互作用的两亲性物质使其相容。在SFME测试和结果的临界分析后,只要加入足够数量的1-辛醇:1-丙醇(3:10 v/v),无论所研究的油水比如何,都可以观察到清晰均匀的微乳液。基于已建立的稳健工作范围,选择1:2(油:超纯水)比(% w/w)作为折衷条件,在保证与色谱系统相容性的同时,最大限度地减少药用油的使用。采用ZORBAX Eclipse Plus C18色谱柱,对色谱条件进行单因素优化,可在35℃条件下同时分析五种大麻素,包括大麻二酚(CBD)、大麻二酸(CBDA)、四氢大麻酚(THCB)、大麻酚(CBN)和四氢大麻酚(Δ9-THC)。方法采用等容洗脱,流动相为82:18 %v/v甲醇:超纯水(含0.15 ± 0.05 % v/v甲酸),流速1.0 mL min−1,进样量20 μL,荧光和紫外吸收检测器。该方案提供了灵敏度(LOD在ng mL−1),选择性和分离效率,与低成本,最小的废物产生和低能源需求相关联,符合绿色化学原则。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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