摘要
目的:建立一种气相色谱-质谱联用仪(GC-MS)技术-同位素内标法(内标物:四氢大麻酚-D_(3),THC-D_(3))同时测定汉麻中大麻二酚(cannabidiol,CBD)、四氢大麻酚(tetrahydrocannabinol,THC)和大麻酚(cannabinol,CBN)3个有效成分的含量,并探讨不同产地汉麻中其含量特征及化学表型。方法:用甲醇超声提取样品中目标成分,离心后制备样品溶液。利用GC-MS,选定合理的色谱、质谱条件,运用同位素内标法建立测定汉麻中CBD、THC、CBN 3个成分含量的定性、定量分析方法。选择的定性定量离子对分别为:CBD,m/z 231→238/314;THC-D_(3),m/z 302→234/317;THC,m/z 299→231/314;CBN,m/z 295→238/310。结果:通过方法学考察得出:3个成分质量浓度在0.2~32.0μg·mL^(-1)范围内线性关系良好(r=0.9996~0.9999),加样回收率为93.2%~112.7%,检测下限(LOD)为0.0023~0.0062μg·mL^(-1),定量下限(LOQ)为0.0076~0.021μg·mL^(-1),精密度,重复性良好,48 h内稳定性较好。18个批次样品测定结果显示:云南昆明和甘肃陇西的CBD含量较高(1.24%~3.43%);内蒙古集宁的THC含量较高,达到0.20%~0.29%,接近毒品型大麻(THC含量>0.3%)的临界值;而黑龙江青冈产地的汉麻样品中,3个成分含量最低。结论:本研究所采用的测定方法可同时检测汉麻中3个有效成分的含量,操作简便易行,专属性高,灵敏高效且结果准确可靠。通过分析探讨3个成分在不同产地含量分布特征及化学表型,得出其含量特征差异性明显,18批次样品初步判断为纤维型大麻。
Objective:To establish a gas chromatography-mass spectrometry(GC-MS)-isotope internal standard method for the simultaneous determination of three active components[cannabidiol(CBD),tetrahydrocannabinol(THC)and cannabinol(CBN)]in hemp,and to explore their content characteristics and chemicalphenotypes in hemp from different habitats.Methods:The target component was extracted by ultrasonic extraction with methanol,and the sample solution was prepared after centrifugation.GC-MS was used to determine the contents of THC,CBN and CBD in hemp by using isotope internal standard method under reasonable chromatographic and mass spectrometry conditions.The selected qualitative and quantitative ion pairs were as follows:CBD,m/z 231→238/314;THC-D_(3),m/z 302-234/317;THC,m/z 299-231/314;CBN,m/z 295-238/310.Results:The three components had a good linear relationship,and the correlation coefficients(r)were 0.9996~0.9999 in the range of 0.2-32.0μg·mL^(-1),the recoveries were 93.2%-112.7%,the lower limit of detections(LODs)were 0.0023-0.0062μg·mL^(-1),the lower limit of quantitation(LOQs)were 0.0076-0.021μg·mL^(-1),the precision and reproducibility were good,and the stability was good within 48 h.The results of 18 batches of samples showed that the CBD contents of Kunming in Yunnan Province and Longxi in Gansu Province were higher(1.24%-3.43%),the THC contents of Jining in Inner Mongolia were higher(0.20%-0.29%),close to the critical value of drug cannabis(THC content>0.3%),and the hemp samples from Heilongjiang Cyclophanthus had the lowest contents of the three components.Conclusion:The method used in this study could simultaneously determine the contents of three active components in hemp.It was easy to operate,specific,sensitive and efficient,and the results were accurate and reliable.By analyzing and discussing the content distribution characteristics and chemical phenotypes of the three components in different areas.It was concluded that the content characteristics were significantly different,and 18 batches of sample
作者
李智宁
魏悦
李飞飞
张丽先
张桃桃
宋梦娇
李自红
LI Zhi-ning;WEI Yue;LI Fei-fei;ZHANG Li-xian;ZHANG Tao-tao;SONG Meng-jiao;LI Zhi-hong(Henan Napu Biotechnology Co.,Ltd.,Henan Academy of Sciences,Zhengzhou 450002,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2021年第11期1894-1903,共10页
Chinese Journal of Pharmaceutical Analysis
基金
河南省科学院科研开发项目(200613051,210913009)
河南省科学院重大科研聚焦项目(190113004,190114002)。
关键词
汉麻
大麻二酚
四氢大麻酚
大麻酚
GC-MS技术
同位素内标法
方法学验证
化学表型
hemp
cannabidiol
tetrahydrocannabinol
cannabinol
GC-MS technology
isotopic internal standard method
methodology validation
chemical phenotype
