超高效液相色谱-串联质谱法分析测定食用植物油中痕量Δ9-四氢大麻酚

Determination of THC in Edible Vegetable Oil by Ultra-high Performance Liquid Chrmatography-Electrospray Tandem Mass Spectrometry

以电喷雾离子源(ESI)为电离源,在负离子采集模式下建立食用植物油中Δ9四氢大麻酚(Δ9-THC)超高效液相色谱-质谱/质谱(UPLC-MS/MS)检测方法。实验以甲醇为提取剂,经中性氧化铝固相萃取柱净化、WatersACQUITYTM UPLC BEH-C18(2.1mm×100mm,1.7μm)色谱柱分离后以UPLC-MS/MS多反应监测模式进行分析。方法检出限和定量限分别为0.15μg/kg和0.45μg/kg。实验以Δ9-氘代四氢大麻酚(Δ9-THC-D3)为内标物,采用内标法定量。3个添加水平,平均回收率为68.0%～110.0%,相对标准偏差为8.8%～18.1%。本方法能够满足食用植物油中Δ9-四氢大麻酚痕量检测的要求。

A determination method for Δ9-tetrahydrocannabinol（THC） in edible vegetable oil was developed on the basis of ultra-high performance liquid chrmatography-electrospray tandem mass spectrometry（UPLC-MS/MS） under negative ion mode using electrospray ionization（ESI） source.THC was extracted with methanol and then purified by LC-alumina-N solid phase extraction column.Qualitative and quantitative analysis were carried out for the analyte under a MRM mode after THC was separated on Waters ACQUITY UPLCTM BEH C18（1.7 μm,2.1 mm × 100 mm） column.The limit of detection（LOD） of the developed method was 0.15 μg/kg and the limit of quantification（LOQ） was 0.45 μg/kg for THC.Quantitative analysis was corrected by internal standard method using delta 9-THC-D3 as internal standard.Average recovery rate of THC varied from 68.0%-110.0% with relative standard deviation ranging from 8.8%-18.1% at three spiked levels.Therefore,the developed method meets the requirements for the determination of THC in edible vegetable oil.