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作 者:次仁曲宗 罗禹[1] 屈晓宇 邓小宽 王永立 高平[1] CIREN Qu-Zong;LUO Yu;QU Xiao-Yu;DENG Xiao-Kuan;WANG Yong-Li;GAO Ping(Key Labortatory Bio-resources and Eco-environment of Ministry Education,College of Life Sciences,Sichuan University,Chengdu 610065,China;Heilongjiang Kangyuan Biotechnology Do.Ltd,Suihua 151600,China)
机构地区:[1]四川大学生命科学学院生物资源与生态环境教育部重点实验室,成都610065 [2]黑龙江康源生物科技有限公司,绥化151600
出 处:《四川大学学报(自然科学版)》2019年第5期957-962,共6页Journal of Sichuan University(Natural Science Edition)
基 金:四川大学横向合作项目(17H0745)
摘 要:研究黑龙江汉麻叶中相关化学成分,建立大麻二酚(CBD)含量检测方法.采用硅胶柱色谱、C18反相中压柱及半制备色谱对汉麻叶乙酸乙酯提取物进行分离纯化,得到5个单体化合物,经核磁NMR解析确定结构为:大麻二酚(CBD)、大麻萜酚(CBG)、大麻酚(CBN)、Δ9-四氢大麻酚酸(Δ9-THCA)、大麻色烯(CBC);以石油醚-二氯甲烷(1∶1)为展开剂,采用碘和1%香草醛乙醇-硫酸(10∶1)分别显色,建立了CBD薄层色谱(TLC)检测方法;以乙腈-0.05%磷酸溶液(80∶20)为流动相,选择CBD吸收峰较高的检测波长,建立了CBD高效液相色谱(HPLC)检测方法;该方法在3.125~100μg/mL线性关系良好(R^2=0.9997),平均回收率为103.69%,RSD 1.32%(n=5).The purpose of this research is to study the chemical constituents in the leaves of Heilongjiang han hemp and establish a method for the determination of cannabidiol(CBD).The ethyl acetate extract of hemp leaf was separated and purified by silica gel column chromatography,C18 reverse phase medium-voltage column and semi preparative chromatography to obtain 5 monomer compounds.And the structure of these compounds was determined by nuclear magnetic(NMR)analysis.They were cannabidiol(CBD),cannabigerol(CBG),cannabinol(CBN),Δ9-Tetrahydrocannabinolic acid(Δ9-THCA)and cannabichromene(CBC).By using petroleum ether-dichloromethane(1∶1)as the developing solvent,iodine and 1%Vanillin ethanol-sulfuric acid(10∶1)were used to establish the TLC method for CBD respectively.High-performance liquid chromatography(HPLC)detection method for CBD was also established by using acetonitrile-0.05%phosphoric acid solution(80∶20)as mobile phase and selecting the detection wavelength with high CBD absorption peak,which has a good linear relationship at 3.125~100 0x0E?SymbolmA@0x0Fg/mL(R 2=0.9997),the average recovery rate is 103.69%and RSD is 1.32%(n=5).
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