摘要
目的:建立同时测定火麻仁中大麻二酚、大麻酚、Δ9-四氢大麻酚含量的方法。方法:采用硅胶柱层析-反相高效液相色谱(RP-HPLC)法。以氯仿-石油醚(4∶1)混合溶剂为淋洗剂,将火麻仁甲醇提取物用硅胶柱层析法纯化处理后,进入HPLC系统进行分析。色谱柱为AgilentZORBAXEclipseXDB-C18(150mm×4.6mm,5μm),流动相为乙腈-水(68∶32),流速为1.0mL·min-1,检测波长为220nm,柱温为30℃。结果:经硅胶柱纯化后,3种大麻酚类物质均能顺利检出。大麻二酚、大麻酚和Δ9-四氢大麻酚的进样量分别在0.02~0.50μg(r=0.9997)、0.01~0.25μg(r=0.9995)和0.01~0.25μg(r=0.9995)范围内与各自峰面积积分值呈良好线性关系;平均加样回收率分别为99.2%、97.6%、97.3%,RSD分别为2.26%、1.93%、2.19%(n均为6)。结论:本法简便、准确、分离度和重复性好,适用于火麻仁的质量控制。
OBJECTIVE:To develop a method for simultaneous determination of cannabidiol,cannabinol and Δ9-tetrehydrocannabinol in Cannabis sativa.METHODS:Silica gel column chromatography-RP-HPLC method was adopted.The methanol extract of C.sativa was purified using silica gel column chromatography,eluted with chloroform-petroleum ether(4 :1).The purified elution was applied to a HPLC system for separation and determination of cannabinoids.The chromatography was carried out on an Agilent ZORBAX Eclipse XDB-C18(150 mm×4.6 mm,5 μm) column with acetonitrile-water(68 :32) as mobile phase at a flow rate of 1.0 mL·min-1.The detection wavelength was set at 220 nm and column temperature was 30 ℃.RESULTS:3 cannabinoids could be successfully determined after purification.The linear ranges of cannabidiol,cannabinol and Δ9-tetrehydrocannabinol were 0.02~0.50 μg(r=0.999 7),0.01~0.25 μg(r=0.999 5) and 0.01~0.25 μg(r=0.999 5),respectively.The average recoveries were 99.2%,97.6%,97.3%,and RSDs were 2.26%,1.93%,2.19%,respectively(n=6).CONCLUSION:The method is simple,accurate,reliable,well-separated and reproducible for the quality control of C.sativa.
出处
《中国药房》
CAS
CSCD
北大核心
2011年第27期2557-2560,共4页
China Pharmacy
基金
辽宁省高等学校科研项目(2008450)
辽宁中医药大学优秀青年药学人才基金(yxrc0912)