黑龙江汉麻叶中化学成分研究与大麻二酚(CBD)含量测定

Study on chemical constituents and determination of cannabidiol (CBD) in hemp leaves of Heilongjiang province

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).