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采用气相色谱/质谱联用技术分析大麻中的萜类化合物:方法开发、验证及应用

Analysis of Terpenes in Cannabis sativa L. Using GC/MS: Method Development, Validation, and Application.

作者信息

Ibrahim Elsayed A, Wang Mei, Radwan Mohamed M, Wanas Amira S, Majumdar Chandrani G, Avula Baharthi, Wang Yan-Hong, Khan Ikhlas A, Chandra Suman, Lata Hemant, Hadad Ghada M, Abdel Salam Randa A, Ibrahim Amany K, Ahmed Safwat A, ElSohly Mahmoud A

机构信息

National Center for Natural Products Research, University of Mississippi, University, MS, USA.

Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Suez Canal University, Ismailia, Egypt.

出版信息

Planta Med. 2019 Mar;85(5):431-438. doi: 10.1055/a-0828-8387. Epub 2019 Jan 15.

DOI:10.1055/a-0828-8387
PMID:30646402
Abstract

Terpenes are the major components of the essential oils present in various L. varieties. These compounds are responsible for the distinctive aromas and flavors. Besides the quantification of the cannabinoids, determination of the terpenes in strains could be of importance for the plant selection process. At the University of Mississippi, a GC-MS method has been developed and validated for the quantification of terpenes in cannabis plant material, viz., -pinene, -pinene, myrcene, limonene, terpinolene, linalool, -terpineol, -caryophyllene, -humulene, and caryophyllene oxide. The method was optimized and fully validated according to AOAC (Association of Official Analytical Chemists) guidelines against reference standards of selected terpenes. Samples were prepared by extraction of the plant material with ethyl acetate containing -tridecane solution (100 µg/mL) as the internal standard. The concentration-response relationship for all analyzed terpenes using the developed method was linear with values > 0.99. The average recoveries for all terpenes in spiked indoor cultivated samples were between 95.0 - 105.7%, with the exception of terpinolene (67 - 70%). The measured repeatability and intermediate precisions (% relative standard deviation) in all varieties ranged from 0.32 to 8.47%. The limit of detection and limit of quantitation for all targeted terpenes were determined to be 0.25 and 0.75 µg/mL, respectively. The proposed method is highly selective, reliable, and accurate and has been applied to the simultaneous determination of these major terpenes in the biomass produced by our facility at the University of Mississippi as well as in confiscated marijuana samples.

摘要

萜类化合物是各种大麻品种中精油的主要成分。这些化合物赋予了大麻独特的香气和风味。除了对大麻素进行定量分析外,测定大麻品种中的萜类化合物对于植物筛选过程也可能具有重要意义。密西西比大学已开发并验证了一种气相色谱 - 质谱(GC-MS)方法,用于定量大麻植物材料中的萜类化合物,即α-蒎烯、β-蒎烯、月桂烯、柠檬烯、萜品油烯、芳樟醇、α-萜品醇、β-石竹烯、α-葎草烯和石竹烯氧化物。该方法根据美国官方分析化学家协会(AOAC)的指南,针对选定萜类化合物的参考标准进行了优化和全面验证。样品通过用含有十三烷溶液(100 µg/mL)作为内标的乙酸乙酯萃取植物材料来制备。使用所开发方法对所有分析的萜类化合物的浓度 - 响应关系呈线性,相关系数>0.99。加标室内种植样品中所有萜类化合物的平均回收率在95.0 - 105.7%之间,但萜品油烯除外(67 - 70%)。所有品种中测得的重复性和中间精密度(相对标准偏差百分比)范围为0.32%至8.47%。所有目标萜类化合物的检测限和定量限分别确定为0.25和0.75 µg/mL。所提出的方法具有高度选择性、可靠性和准确性,已应用于同时测定密西西比大学我们实验室生产的大麻生物质以及没收的大麻样品中的这些主要萜类化合物。

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