UPLC-MS/MS同时测定四种食品基质中痕量四氢大麻酚、大麻二酚和大麻酚

Determination of Tetrahydrocannabinol, Cannabidiol and Cannabinol in Four Food Matrices by Ultra Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry

摘要:

建立了UPLC-MS/MS同时测定食品中痕量四氢大麻酚、大麻二酚、大麻酚3种大麻素的检测方法，样品经甲醇提取，提取液过HLB固相萃取柱净化，经过Athena C18-WP色谱柱（2.1×150 mm，3 μm）分离，以甲醇-水流动相梯度洗脱，电喷雾负离子扫描，多反应监测模式检测。以基质配标法消除基质效应，THC-D3内标法定量。该方法在0~10 μg/L浓度范围内线性相关系数（r2）大于0.999。大麻二酚（Cannabidiol，CBD）和大麻酚（Cannabinol，CBN）的LOD为0.03 μg/kg，LOQ为0.1 μg/kg。四氢大麻酚（Tetrahydrocannabinol，THC）的LOD为0.15 μg/kg，LOQ为0.5 μg/kg。考察了三种大麻素在四种不同食品基质中的加标回收率，在1 LOQ、5 LOQ、10 LOQ的加标水平下，三种大麻素的加标回收率为81.1%~114.7%。相对标准偏差（RSD）为0.25%~4.63%（n=6）。结果表明，该方法稳定性好、灵敏度高，适用于常见食品基质中三种大麻素的同时测定。

Abstract:

A method for the simultaneous determination of trace amounts of tetrahydrocannabinol, cannabidiol and cannabinoids in food by UPLC-MS/MS was developed. The sample was purified by methanol and the extract was purified by HLB solid phase extraction column. Athena C18- WP column (2.1×150 mm, 3 μm) was used to separatethe samples. The methanol-water was used as mobile phase gradient. The electrospray negative ion scanning and multiple reaction monitoring mode detection were employed. Matrix effects were eliminated by matrix labeling and quantified by THC-D3 internal standard method. The linear correlation coefficient (r2) of this method was greater than 0.999 in the concentration range of 0~10 μg/L. Cannabisdiol (CBD) and cannabinol (CBN) had an LOD of 0.03 μg/kg and an LOQ of 0.1 μg/kg. Tetrahydrocannabinol (THC) had an LOD of 0.15 μg/kg and an LOQ of 0.5 μg/kg. The spiked recoveries of three cannabinoids in four different food matrices were investigated. Under the spiked levels of LOQ, 5 LOQ and 10 LOQ, the spiked recoveries of the three cannabinoids ranged from 81.1% to 114.7%. The relative standard deviation (RSD) was 0.25% to 4.63% (n=6). The results showed that the method had good stability and high sensitivity, and was suitable for simultaneous determination of three cannabinoids in common food matrices.