固相萃取柱的制备及其与超高效液相色谱联用测定工业大麻中3种大麻酚  

Preparation of a solid phase extraction column and the determination of three cannabinol compounds in industrial hemp by combining with UPLC

作　　者：李少华 申书昌[1] 杨雪 于轩恒 杨铂玮 LI Shaohua;SHEN Shuchang;YANG Xue;YU Xuanheng;YANG Bowei(Center of Analytical and Testing,Qiqihar University,Qiqihar 161006)

机构地区：[1]齐齐哈尔大学分析测试中心,齐齐哈尔161006

出　　处：《分析试验室》2021年第5期578-582,共5页Chinese Journal of Analysis Laboratory

基　　金：黑龙江省教育厅基本科研业务专项(135209221)项目资助。

摘　　要：将中性氧化铝、硅酸镁和石墨化炭黑混合后,填加于聚丙烯管中制成固相萃取柱,对工业大麻花叶的乙酸乙酯-甲醇提取液进行了净化处理,采用超高效液相色谱法(UPLC)测定了净化液中大麻二酚(CBD)、大麻酚(CBN)和Δ9-四氢大麻酚(Δ9-THC)的含量。考察了中性氧化铝、硅酸镁和石墨化炭黑对提取液中色素、总糖、总脂肪酸酯及金属离子等杂质的吸附性能,确定了3种吸附剂的最佳配比。将自制小柱与石墨化炭黑/氨基(CARB/NH2)柱的性能进行了对比。选择了液相色谱条件,在0.5~50 mg/L范围内,CBD,CBN,Δ9-THC的峰面积与浓度呈良好的线性关系,3种植大麻酚的检出限分别为0.45,0.53,0.38μg/L;回收率分别为94.6%~103.4%,95.7%~99.7%,97.4%~104.1%;相对标准偏差(RSD)分别为2.1%~3.6%,2.4%~4.7%,3.9%~5.4%。A solid phase extraction column was prepared by filling the mixture of neutral alumina,magnesium silicate and graphitized carbon black into polypropylene tube.Three cannabinol compounds from hemp’s flowers and leaves were extracted by mixed solution(ethyl acetate and methanol)and the obtained solid phase extraction column was used to purify the extracting solution.Meanwhile,the concentrations of cannabidiol(CBD),cannabinol(CBN)andΔ9-tetrahydrocannabinol(Δ9-THC)in the solution were determined by ultra performance liquid chromatography(UPLC).In addition,the adsorption performances of neutral alumina,magnesium silicate and graphitized carbon black to pigments,total sugar,total fatty glyceride and metal ions were investigated,then the optimum ratio of the three adsorbents was selected.There were good linear relationships between peak areas of CBD,CBN andΔ9-THC and concentrations in the range of 0.5-50 mg/L.The detection limits of three cannabinol compounds were 0.45,0.53,0.38μg/L,respectively,the recoveries were 94.6%-103.4%,95.7%-99.7%,97.4%-104.1%and the relative standard deviations(RSD)were 2.1%-3.6%,2.4%-4.7%,3.9%-5.4%,respectively.

关 键 词：固相萃取柱 中性氧化铝 硅酸镁 石墨化炭黑 超高效液相色谱 工业大麻 

分 类 号：O658.2[理学—分析化学]